Conversion of Carbon Dioxide to Ethanol by Electrochemical Synthesis Method Using Brass as A Cathode

Directory of Open Access Journals (Sweden)

Septian Ramadan

2017-09-01

Full Text Available The effect of potential and gas flow rate were investigated to determine the optimum conditions of the electrochemical synthesis process to convert carbon dioxide to ethanol. The conversion process is carried out using a NaHCO3 electrolyte solution in an electrochemical reactor equipped with a cathode and anode. As cathode is used brass, while as anode is used carbon. The result of the electrochemical synthesis process was analyzed by gas chromatography to determine the content of the compounds produced qualitatively and quantitatively. The optimum electrochemical synthesis conditions to convert carbon dioxide to ethanol are potential and gas flow rate are 3 volts and 0.5 L/minutes with ethanol concentration yielded 1.32%.

Electrochemically Active Biofilms Assisted Nanomaterial Synthesis for Environmental Applications

KAUST Repository

Ahmed, Elaf

2017-01-01

Nanomaterials have a great potential for environmental applications due to their high surface areas and high reactivity. This dissertation investigated the use of electrochemically active biofilms (EABs) as a synthesis approach for the fabrication

Synthesis and characterization of poly aniline for electrochemical biosensor construction

International Nuclear Information System (INIS)

Magalhaes, Gleice S.L.; Southgate, Erica F.; Alhadeff, Eliana M.; Guimaraes, Maria Jose O.C.

2011-01-01

Conductors polymers have many attractive interests to the industry due their highly technological applications. This work treats specially of polyaniline because it's large electrical conductivity, electrochemical properties, associate to the chemical stability in environmental conditions and synthesis facility. The main of this work is the application in a construction of an electrochemical biosensor for ethanol detection and quantification. Different conditions of synthesis of the conductor emeraldine polyaniline form were studied, investigated the influence of the dopant agent and the reactional environment conditions temperature on the reaction yield and conductivities. The polyaniline that showed the best conductivity were characterized by differential and thermal gravimetric analysis, infrared spectroscopy, X ray diffraction, and cycle voltammetry, comparing with the commercial polyaniline. (author)

Conversion of Carbon Dioxide into Ethanol by Electrochemical Synthesis Method Using Cu-Zn Electrode

Science.gov (United States)

Riyanto; Ramadan, S.; Fariduddin, S.; Aminudin, A. R.; Hayatri, A. K.

2018-01-01

Research on conversion of carbon dioxide into ethanol has been done. The conversion process is carried out in a sodium bicarbonate electrolyte solution in an electrochemical synthesis reactor. As cathode was used Cu-Zn, while as anode carbon was utilized. Variations of voltage, concentration of sodium bicarbonate electrolyte solution and time of electrolysis were performed to determine the optimum conditions to convert carbon dioxide into ethanol. Sample of the electrochemical synthesis process was analyzed by gas chromatography. From the result, it is found that the optimum conditions of the electrochemical synthesis process of carbon dioxide conversion into ethanol are voltage, concentration of sodium bicarbonate electrolyte solution and time of electrolysis are 3 volts, 0.4 M and 90 minutes with the ethanol concentration of 10.44%.

Synthesis and utilization of carbon nanotubes for fabrication of electrochemical biosensors

International Nuclear Information System (INIS)

Lawal, Abdulazeez T.

2016-01-01

Graphical abstract: Carbon nanotubes. - Highlights: • This review discusses synthesis and applications of carbon nanotubes sensors. • The review summarizes contributions of carbon nanotube to electrochemical biosensor. • Good electrical conductivity makes carbon nanotubes a good material for biosensors. • Carbon nanotubes promotes electron transfer that aids biosensing of biomolecules. - Abstract: This review summarizes the most recent contributions in the fabrication of carbon nanotubes-based electrochemical biosensors in recent years. It discusses the synthesis and application of carbon nanotubes to the assembly of carbon nanotube-based electrochemical sensors, its analytical performance and future expectations. An increasing number of reviews and publications involving carbon nanotubes sensors have been reported ever since the first design of carbon nanotube electrochemical biosensors. The large surface area and good electrical conductivity of carbon nanotubes allow them to act as “electron wire” between the redox center of an enzyme or protein and an electrode's surface, which make them very excellent material for the design of electrochemical biosensors. Carbon nanotubes promote the different rapid electron transfers that facilitate accurate and selective detection of cytochrome-c, β-nicotinamide adenine dinucleotide, hemoglobin and biomolecules, such as glucose, cholesterol, ascorbic acid, uric acid, dopamine pesticides, metals ions and hydrogen peroxide.

Synthesis and utilization of carbon nanotubes for fabrication of electrochemical biosensors

Energy Technology Data Exchange (ETDEWEB)

Lawal, Abdulazeez T., E-mail: abdul.lawal@yahoo.com

2016-01-15

Graphical abstract: Carbon nanotubes. - Highlights: • This review discusses synthesis and applications of carbon nanotubes sensors. • The review summarizes contributions of carbon nanotube to electrochemical biosensor. • Good electrical conductivity makes carbon nanotubes a good material for biosensors. • Carbon nanotubes promotes electron transfer that aids biosensing of biomolecules. - Abstract: This review summarizes the most recent contributions in the fabrication of carbon nanotubes-based electrochemical biosensors in recent years. It discusses the synthesis and application of carbon nanotubes to the assembly of carbon nanotube-based electrochemical sensors, its analytical performance and future expectations. An increasing number of reviews and publications involving carbon nanotubes sensors have been reported ever since the first design of carbon nanotube electrochemical biosensors. The large surface area and good electrical conductivity of carbon nanotubes allow them to act as “electron wire” between the redox center of an enzyme or protein and an electrode's surface, which make them very excellent material for the design of electrochemical biosensors. Carbon nanotubes promote the different rapid electron transfers that facilitate accurate and selective detection of cytochrome-c, β-nicotinamide adenine dinucleotide, hemoglobin and biomolecules, such as glucose, cholesterol, ascorbic acid, uric acid, dopamine pesticides, metals ions and hydrogen peroxide.

Electrochemical synthesis and characterization of copper (I oxide

Directory of Open Access Journals (Sweden)

Bugarinović Sanja J.

2009-01-01

Full Text Available The quest and need for clean and economical energy sources have increased interest in the development of thin film cells technologies. Electrochemical deposition is an attractive method for synthesis of thin films. It offers the advantages of low synthesis temperature, low cost and high purity. Copper (I oxide or cuprous oxide is an oxide semiconductor which is used as the anodic material in the form of thin film in lithium batteries and solar cells. The cathodic process of synthesis of cuprous oxide thin film is carried out in a potentiostatic mode from the organic electrolyte. The process parameters are chosen in that way to accomplish maximum difference between the potentials at which Cu2O and CuO are obtained. The electrochemical characterization was carried out by cyclic voltammetry. The electrodeposition techniques are particularly well suited for the deposition of single elements but it is also possible to carry out simultaneous depositions of several elements and syntheses of well-defined alternating layers of metals and oxides with thicknesses down to a few nm. Nanomaterials exhibit novel physical properties and play an important role in fundamental research. In addition, cuprous oxide is commonly used as a pigment, a fungicide, and an antifouling agent for marine paints. It is insoluble in water and organic solvents. This work presents the examinations of the influence of bath, temperature, pH and current density on the characteristics of electrochemically synthesized cuprous oxide. In the 'classic' process of synthesis, which is carried out under galvanostatic conditions on the anode, the grain size of the powder decreases with the increase in current density while the grain colour becomes lighter. The best commercial quality of the Cu2O (grain size, colour, content of choride was obtained at the temperature of 80°C, concentration of NaCl of 3 mol/dm3 and current density of 400 A/m2.

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

Science.gov (United States)

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.

Electrochemical Synthesis of Ammonia from Water and Nitrogen using a Pt/GDC/Pt Cell

International Nuclear Information System (INIS)

Kim, Jong Nam; Yoo, Chung-Yul; Joo, Jong Hoon; Yu, Ji Haeng; Sharma, Monika; Yoon, Hyung Chul; Jeoung, Hana; Song, Ki Chang

2014-01-01

Electrochemical ammonia synthesis from water and nitrogen using a Pt/GDC/Pt cell was experimentally investigated. Electrochemical analysis and ammonia synthesis in the moisture-saturated nitrogen environment were performed under the operating temperature range 400-600 .deg. C and the applied potential range OCV (Open Circuit Voltage)-1.2V. Even though the ammonia synthesis rate was augmented with the increase in the operating temperature (i.e.. increase in the applied current) under the constant potential, the faradaic efficiency was decreased because of the limitation of dissociative chemisorption of nitrogen on the Pt electrode. The maximum synthesis rate of ammonia was 3.67x10 -11 mols -1 cm -2 with 0.1% faradaic efficiency at 600 .deg. C

Direct electrochemical synthesis of metal alcoholates

International Nuclear Information System (INIS)

Shrejder, V.A.; Turevskaya, E.P.; Kozlova, N.I.; Turova, N.Ya.

1981-01-01

Conditions of electrochemical synthesis of Ga, Sc, Y, Ge, Ti, Zr, Nb and Ta alcoholates during anodic metal dissolution in absolute alcohols in the presence of background electrolyte are studied. R 4 NBr and R 4 NBF 4 salts are optimum background electrolytes. Application limits of this synthetical method using different metals as anode are determined. It is supposed that alkoxyhalogenides the nature of which determines further direction of electrode process, are the primary products of anodic oxidation of metals [ru

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

Directory of Open Access Journals (Sweden)

Yuta Isoda

2017-05-01

Full Text Available 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.

Spectral characterization of a newly synthesized fluorescent semicarbazone derivative and its usage as a selective fiber optic sensor for copper(II).

Science.gov (United States)

Oter, Ozlem; Ertekin, Kadriye; Kirilmis, Cumhur; Koca, Murat

2007-02-19

In this work photoluminescent properties of highly Cu(2+) selective organic fluoroionophore, semicarbazone derivative; bis(naphtho[2,1-b]furan-2-yl)methanone semicarbazone (BNF) was investigated in different solvents (dichloromethane, tetrahydrofuran, toluene and ethanol) and in polymer matrices of polyvinylchloride (PVC) and ethyl cellulose (EC) by absorption and emission spectrometry. The BNF derivative displayed enhanced fluorescence emission quantum yield, Q(f)=6.1 x 10(-2) and molar extinction coefficient, epsilon=29,000+/-65 cm(-1)M(-1) in immobilized PVC matrix, compared to 2.6 x 10(-3) and 24,573+/-115 in ethanol solution. The offered sensor exhibited remarkable fluorescence intensity quenching upon exposure to Cu(2+) ions at pH 4.0 in the concentration range of 1.0 x 10(-9) to 3.0 x 10(-4)M [Cu(2+)] while the effects of the responding ions (Ca(2+), Hg(+), Pb(2+), Al(3+), Cr(3+), Mn(2+), Mg(2+), Sn(2+), Cd(2+), Co(2+) and Ni(2+)) were less pronounced.

Electrochemical oxidation of 4-morpholinoaniline in aqueous solutions: Synthesis of a new trimer of 4-morpholinoaniline

International Nuclear Information System (INIS)

Esmaili, Roya; Nematollahi, Davood

2011-01-01

Research highlights: → Electrochemical study of 4-morpholinoaniline in various pHs. → Electrochemical trimerization of 4-morpholinoaniline in aqueous solution. → Green method for the synthesis of '4-morpholinoaniline-trimer'. → Potential-pH diagram for 4-morpholinoaniline. - Abstract: Electrochemical oxidation of 4-morpholinoaniline has been studied in various pHs using cyclic voltammetry and controlled-potential coulometry. The electrochemical trimerization of 4-morpholinoaniline is described and its mechanism has been studied in aqueous solution. This method provides a green, reagent-less, and environmentally friendly procedure with high atom economy, for the synthesis of '4-morpholinoaniline-trimer' using a carbon electrode in an undivided cell in good yield and purity.

Electrochemical Synthesis of Ammonia from Water and Nitrogen using a Pt/GDC/Pt Cell

Energy Technology Data Exchange (ETDEWEB)

Kim, Jong Nam; Yoo, Chung-Yul; Joo, Jong Hoon; Yu, Ji Haeng; Sharma, Monika; Yoon, Hyung Chul [Korea Institute of Energy Research, Daejeon (Korea, Republic of); Jeoung, Hana; Song, Ki Chang [Konyang University, Nonsan (Korea, Republic of)

2014-02-15

Electrochemical ammonia synthesis from water and nitrogen using a Pt/GDC/Pt cell was experimentally investigated. Electrochemical analysis and ammonia synthesis in the moisture-saturated nitrogen environment were performed under the operating temperature range 400-600 .deg. C and the applied potential range OCV (Open Circuit Voltage)-1.2V. Even though the ammonia synthesis rate was augmented with the increase in the operating temperature (i.e.. increase in the applied current) under the constant potential, the faradaic efficiency was decreased because of the limitation of dissociative chemisorption of nitrogen on the Pt electrode. The maximum synthesis rate of ammonia was 3.67x10{sup -11} mols{sup -1}cm{sup -2} with 0.1% faradaic efficiency at 600 .deg. C.

Nickel-cobalt hydroxide nanosheets: Synthesis, morphology and electrochemical properties.

Science.gov (United States)

Schneiderová, Barbora; Demel, Jan; Zhigunov, Alexander; Bohuslav, Jan; Tarábková, Hana; Janda, Pavel; Lang, Kamil

2017-08-01

This paper reports the synthesis, characterization, and electrochemical performance of nickel-cobalt hydroxide nanosheets. The hydroxide nanosheets of approximately 0.7nm thickness were prepared by delamination of layered nickel-cobalt hydroxide lactate in water and formed transparent colloids that were stable for months. The nanosheets were deposited on highly oriented pyrolytic graphite by spin coating, and their electrochemical behavior was investigated by cyclic voltammetry in potassium hydroxide electrolyte. Our method of electrode preparation allows for studying the electrochemistry of nanosheets where the majority of the active centers can participate in the charge transfer reaction. The observed electrochemical response was ascribed to mutual compensation of the cobalt and nickel response via electron sharing between these metals in the hydroxide nanosheets, a process that differentiates the behavior of nickel-cobalt hydroxide nanosheets from single nickel hydroxide or cobalt hydroxide nanosheets or their physical mixture. The presence of cobalt in the nickel-cobalt hydroxide nanosheets apparently decreases the time of electrochemical activation of the nanosheet layer, which for the nickel hydroxide nanosheets alone requires more potential sweeps. Copyright © 2017 Elsevier Inc. All rights reserved.

The Effects of Voltage and Concentration of Sodium Bicarbonate on Electrochemical Synthesis of Ethanol from Carbon Dioxide Using Brass as Cathode

Science.gov (United States)

Ramadan, Septian; Fariduddin, Sholah; Rizki Aminudin, Afianti; Kurnia Hayatri, Antisa; Riyanto

2017-11-01

The effects of voltage and concentration of sodium bicarbonate were investigated to determine the optimum conditions of the electrochemical synthesis process to convert carbon dioxide into ethanol. The conversion process is carried out using a sodium bicarbonate electrolyte solution in an electrochemical synthesis reactor equipped with a cathode and anode. As the cathode was used brass, while as the anode carbon was utilized. Sample of the electrochemical synthesis process was analyzed by gas chromatography to determine the content of the compounds produced. The optimum electrochemical synthesis conditions to convert carbon dioxide into ethanol are voltage and concentration of sodium bicarbonate are 3 volts and 0.4 M with ethanol concentration of 1.33%.

One step paired electrochemical synthesis of iron and iron oxide nanoparticles

Directory of Open Access Journals (Sweden)

Ordoukhanian Juliet

2016-09-01

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

Water-based synthesis of hydrophobic ionic liquids for high-energy electrochemical devices

International Nuclear Information System (INIS)

Montanino, Maria; Alessandrini, Fabrizio; Passerini, Stefano; Appetecchi, Giovanni Battista

2013-01-01

Highlights: ► Water-based synthesis of ionic liquids with high yield. ► Full recycling of reagents. ► High purity pyrrolidinium-based ionic liquids with exceptional electrochemical stability window. ► Lithium plating from pyrrolidinium-based ionic liquids. -- Abstract: In this work is described an innovative synthesis route for hydrophobic ionic liquids (ILs) composed of N-methyl-N-alkylpyrrolidinium (or piperidinium) or imidazolium or tetralkylammonium cations and (perfluoroalkylsulfonyl)imide, ((C n F 2n+1 SO 2 )(C m F 2m+1 SO 2 )N − ), anions. This synthesis does not require the use of any environmental unfriendly solvent such as acetone, acetonitrile or halogen-containing compounds, which is not welcome in industrial applications. Only water is used as the process solvent throughout the entire process. In addition, the commonly used iodine-containing reagents were replaced by the cheaper, more chemically stable and less toxic bromine-containing compounds. A particular care was devoted to the development of the purification route, which is especially important for ILs to be used in high-energy electrochemical devices such as high voltage supercapacitors and lithium batteries. The effect of the reaction temperature, the time and the stoichiometry in the various steps of the synthesis have been investigated in detail. This novel procedure allowed obtaining ultrapure (>99.9 wt.%), clear, colourless, inodorous ILs with an overall yield above 92 wt.% and moisture content below 1 ppm. NMR measurements were run to confirm the chemical structure whereas elemental analysis and electrochemical tests were performed to check the purity of the synthesized ILs

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

International Nuclear Information System (INIS)

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

2012-01-01

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

Synthesis, characterization and electrochemical investigation of hetaryl chromium(0) aminocarbene complexes

Czech Academy of Sciences Publication Activity Database

Metelková, R.; Tobrman, T.; Kvapilová, Hana; Hoskovcová, I.; Ludvík, Jiří

2012-01-01

Roč. 82, SI (2012), s. 470-477 ISSN 0013-4686 R&D Projects: GA AV ČR IAA400400813 Institutional support: RVO:61388955 Keywords : Fischer aminocarbene complexes * synthesis * Electrochemical oxidation and reduction Subject RIV: CG - Electrochemistry Impact factor: 3.777, year: 2012

Electrochemical synthesis of nanosized TiO2 nanopowder involving choline chloride based ionic liquids

International Nuclear Information System (INIS)

Anicai, Liana; Petica, Aurora; Patroi, Delia; Marinescu, Virgil; Prioteasa, Paula; Costovici, Stefania

2015-01-01

Highlights: • TiO 2 nanopowder electrochemically prepared using choline chloride based ionic liquids. • The new proposed method allowed high anodic synthesis efficiencies of minimum 92%. • High surface area of the electrochemically synthesized titania nanopowders. • Enhanced photocatalytic activity. - Abstract: The paper presents some experimental results regarding the electrochemical synthesis of TiO 2 nanopowders through anodic dissolution of Ti metal in choline chloride based eutectic mixtures (DES). A detailed characterization of the obtained titania has been performed, using various techniques, including XRD, Raman spectroscopy, XPS, SEM associated with EDX analysis, BET and UV–vis diffuse reflectance spectra. The anodic behavior of Ti electrode in DES has been also investigated. The photoreactivity of the synthesized materials was evaluated for the degradation of Orange II dye under UV (λ = 365 nm) and visible light irradiation. An anodic synthesis efficiency of minimum 92% has been determined. The as-synthesized TiO 2 showed amorphous structure and a calcination post-treatment at temperatures between 400 and 600 °C yielded anatase. The anodically obtained nanocrystalline oxides have crystallite sizes of 8–18 nm, a high surface area and enhanced photocatalytic effect

Direct on-chip DNA synthesis using electrochemically modified gold electrodes as solid support

Science.gov (United States)

Levrie, Karen; Jans, Karolien; Schepers, Guy; Vos, Rita; Van Dorpe, Pol; Lagae, Liesbet; Van Hoof, Chris; Van Aerschot, Arthur; Stakenborg, Tim

2018-04-01

DNA microarrays have propelled important advancements in the field of genomic research by enabling the monitoring of thousands of genes in parallel. The throughput can be increased even further by scaling down the microarray feature size. In this respect, microelectronics-based DNA arrays are promising as they can leverage semiconductor processing techniques with lithographic resolutions. We propose a method that enables the use of metal electrodes for de novo DNA synthesis without the need for an insulating support. By electrochemically functionalizing gold electrodes, these electrodes can act as solid support for phosphoramidite-based synthesis. The proposed method relies on the electrochemical reduction of diazonium salts, enabling site-specific incorporation of hydroxyl groups onto the metal electrodes. An automated DNA synthesizer was used to couple phosphoramidite moieties directly onto the OH-modified electrodes to obtain the desired oligonucleotide sequence. Characterization was done via cyclic voltammetry and fluorescence microscopy. Our results present a valuable proof-of-concept for the integration of solid-phase DNA synthesis with microelectronics.

The self-assembly of redox active peptides: Synthesis and electrochemical capacitive behavior.

Science.gov (United States)

Piccoli, Julia P; Santos, Adriano; Santos-Filho, Norival A; Lorenzón, Esteban N; Cilli, Eduardo M; Bueno, Paulo R

2016-05-01

The present work reports on the synthesis of a redox-tagged peptide with self-assembling capability aiming applications in electrochemically active capacitive surfaces (associated with the presence of the redox centers) generally useful in electroanalytical applications. Peptide containing ferrocene (fc) molecular (redox) group (Ac-Cys-Ile-Ile-Lys(fc)-Ile-Ile-COOH) was thus synthesized by solid phase peptide synthesis (SPPS). To obtain the electrochemically active capacitive interface, the side chain of the cysteine was covalently bound to the gold electrode (sulfur group) and the side chain of Lys was used to attach the ferrocene in the peptide chain. After obtaining the purified redox-tagged peptide, the self-assembly and redox capability was characterized by cyclic voltammetry (CV) and electrochemical impedance-based capacitance spectroscopy techniques. The obtained results confirmed that the redox-tagged peptide was successfully attached by forming an electroactive self-assembled monolayer onto gold electrode. The design of redox active self-assembly ferrocene-tagged peptide is predictably useful in the development of biosensor devices precisely to detect, in a label-free platform, those biomarkers of clinical relevance. © 2016 Wiley Periodicals, Inc. Biopolymers (Pept Sci) 106: 357-367, 2016. © 2016 Wiley Periodicals, Inc.

Characterization and optimization of cathodic conditions for H2O2 synthesis in microbial electrochemical cells

Science.gov (United States)

Cathode potential and O2 supply methods were investigated to improve H2O2 synthesis in an electrochemical cell, and optimal cathode conditions were applied for microbial electrochemical cells (MECs). Using aqueous O2 for the cathode significantly improved current density, but H2...

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

Science.gov (United States)

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

2012-03-21

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

Electrochemical synthesis of nanosized TiO{sub 2} nanopowder involving choline chloride based ionic liquids

Energy Technology Data Exchange (ETDEWEB)

Anicai, Liana, E-mail: lanicai@itcnet.ro [POLITEHNICA University of Bucharest, Center of Surface Science and Nanotechnology, Splaiul Independentei 313, Bucharest, 060042 (Romania); Petica, Aurora [Leather and Footwear Research Institute (ICPI), Ion Minulescu 93, Bucharest, 031215 (Romania); Patroi, Delia; Marinescu, Virgil; Prioteasa, Paula [INCDIE ICPE-Advanced Research, Splaiul Unirii 313, Bucharest (Romania); Costovici, Stefania [POLITEHNICA University of Bucharest, Center of Surface Science and Nanotechnology, Splaiul Independentei 313, Bucharest, 060042 (Romania)

2015-09-15

Highlights: • TiO{sub 2} nanopowder electrochemically prepared using choline chloride based ionic liquids. • The new proposed method allowed high anodic synthesis efficiencies of minimum 92%. • High surface area of the electrochemically synthesized titania nanopowders. • Enhanced photocatalytic activity. - Abstract: The paper presents some experimental results regarding the electrochemical synthesis of TiO{sub 2} nanopowders through anodic dissolution of Ti metal in choline chloride based eutectic mixtures (DES). A detailed characterization of the obtained titania has been performed, using various techniques, including XRD, Raman spectroscopy, XPS, SEM associated with EDX analysis, BET and UV–vis diffuse reflectance spectra. The anodic behavior of Ti electrode in DES has been also investigated. The photoreactivity of the synthesized materials was evaluated for the degradation of Orange II dye under UV (λ = 365 nm) and visible light irradiation. An anodic synthesis efficiency of minimum 92% has been determined. The as-synthesized TiO{sub 2} showed amorphous structure and a calcination post-treatment at temperatures between 400 and 600 °C yielded anatase. The anodically obtained nanocrystalline oxides have crystallite sizes of 8–18 nm, a high surface area and enhanced photocatalytic effect.

Electrochemical Study of Bromide in the Presence of 1,3-Indandione. Application to the Electrochemical Synthesis of Bromo Derivatives of 1,3-Indandione

OpenAIRE

Nematollahi, D.; Akaberi, N.

2001-01-01

The electrochemical oxidation of bromide in the presence of 1,3-indandione (1) in water/acetic acid and methanol/acetic acid mixtures has been studied by cyclic voltammetry and controlled-potential coulometry. The results indicate the participation of 1,3-indandione in the bromination reaction. On the basis of the electroanalytical and preparative results a reaction mechanism including electron transfer, chemical reaction and regeneration of bromide was discussed. The electrochemical synthesi...

A new inorganic-organic nanohybrid based on a copper(II) semicarbazone complex and the PMo.sub.12./sub.O.sup.3-./sup..sub.40./sub. polyanion: synthesis, characterization, crystal structure and photocatalytic activity for degradation of cationic dyes

Czech Academy of Sciences Publication Activity Database

Farhadi, S.; Mahmoudi, F.; Dušek, Michal; Eigner, Václav; Kučeráková, Monika

2017-01-01

Roč. 122, Jan (2017), s. 247-256 ISSN 0277-5387 R&D Projects: GA ČR(CZ) GA14-03276S; GA MŠk LO1603 EU Projects: European Commission(XE) CZ.2.16/3.1.00/24510 Institutional support: RVO:68378271 Keywords : inorganic-organic hybrid * semicarbazone complex * nanohybrid * photodegradation * cationic dyes Subject RIV: CA - Inorganic Chemistry OBOR OECD: Inorganic and nuclear chemistry Impact factor: 1.926, year: 2016

Electrochemical synthesis of poly(pyrrole-co-o-anisidine)/chitosan composite films

Science.gov (United States)

Yalçınkaya, Süleyman; Çakmak, Didem

2017-05-01

In this study, poly(pyrrole-co-o-anisidine)/chitosan composite films were electrochemically synthesized in various monomers feed ratio (pyrrole: o-anisidine; 9:1, 7:3, 1:1, 3:7 and 1:9) of pyrrole and o-anisidine on the platinum electrode. Electrochemical synthesis of the composite films was carried out via cyclic voltammetry technique. They were characterized by FT-IR, cyclic voltammetry, SEM micrographs, digital images, TGA and DSC techniques. The SEM results indicated that the particle size of the composite decreased with increasing o-anisidine ratio and the films became more likely to be smooth morphology. The TGA results proved that the film of the composite with 1:1 ratio showed highest final degradation temperature and lowest weight loss (83%) compared to copolymer and 9:1 1:9 composite films. The 1:1 composite film had higher thermal stability than copolymer and the other composite films (9:1 1:9). Meanwhile, electrochemical studies exhibited that the 1/9 composite film had good electrochemical stability as well.

Electrochemical synthesis of transition element complexes with carboxyl- and carbonyl-containing ligands

International Nuclear Information System (INIS)

Frolov, V.Yu.; Bolotin, S.N.; Panyushkin, V.T.

2005-01-01

Complexes of d- and f-elements (E = Cu, Ni, Zn, Nd, Tb, Pr, Gd, Er) with carboxyl- and carbonyl-containing ligands were synthesized by the electrochemical method. The products were characterized by elemental analysis, thermal gravimetric analysis and IR spectra. The influence exerted by a number of factors on the process course was studied. The dependence of the electro synthesis parameters on the composition of the forming compounds was established. A new method for anodic synthesis of these compounds was developed [ru

An electrochemical procedure coupled with a Schiff base method; application to electroorganic synthesis of new nitrogen-containing heterocycles

International Nuclear Information System (INIS)

Dowlati, Bahram; Othman, Mohamed Rozali

2013-01-01

The synthesis of Nitrogen-containing heterocycles has been achieved using chemical and electrochemical methods, respectively. The direct chemical synthesis of nucleophiles proceeds through the Schiff base chemical reaction. This procedure offers an alternate reaction between dicarbonyl compounds and diamines leads to the formation of products. The results indicate that the Schiff base chemical method for synthesis of the product has successfully performed in excellent overall yield. In the electrochemical step, a series of Nitrogen-containing compounds were electrosynthesized. Various parameters such as the applied potential, pH of the electrolytic solution, cell configuration and also purification techniques, were carried out to optimize the yields of corresponding products. New Nitrogen-containing heterocycle derivatives were synthesized using an electrochemical procedure coupled with a Schiff base as a facile, efficient and practical method. The products have been characterized after purification by IR, 1 H NMR, 13 C NMR and ESI-MS 2

Facile electrochemical synthesis of few layered graphene from discharged battery electrode and its

Directory of Open Access Journals (Sweden)

Santosh K. Tiwari

2017-05-01

Full Text Available A cost-effective, simple and non-hazardous route for synthesis of few-layered graphene from waste zinc carbon battery (ZCB electrodes via electrochemical expansion (ECE has been reported. In this synthesis, we have electrochemically exfoliated the graphene layers, by intercalating sodium dodecyl benzenesulfonate (SDBS surfactant into graphitic layers at different D.C. voltages with a constant SDBS concentration. The graphene sheets were isolated, purified and characterized by Transmission electron microscopy (TEM, Scanning electron microscopy (SEM, Fourier transform infrared spectrometry (FTIR, X-ray diffraction (XRD, Raman spectrometry, Ultraviolet absorption (UV, Selected area electron diffraction (SAED and Cyclic voltammetry. Best result was obtained at 4.5 V of D.C. A possible mechanism for the intercalation process has been proposed. A promising application of the produced material for supercapacitor application has also been explored in combination with polyaniline.

Spectroscopic evaluation of Co(II), Ni(II) and Cu(II) complexes derived from thiosemicarbazone and semicarbazone

Science.gov (United States)

Chandra, Sulekh; Kumar, Anil

2007-12-01

Co(II), Ni(II) and Cu(II) complexes were synthesized with thiosemicarbazone (L 1) and semicarbazone (L 2) derived from 2-acetyl furan. These complexes were characterized by elemental analysis, molar conductance, magnetic moment, mass, IR, electronic and EPR spectral studies. The molar conductance measurement of the complexes in DMSO corresponds to non-electrolytic nature. All the complexes are of high-spin type. On the basis of different spectral studies six coordinated geometry may be assigned for all the complexes except Co(L) 2(SO 4) and Cu(L) 2(SO 4) [where L = L 1 and L 2] which are of five coordinated square pyramidal geometry.

Water/ionic liquid/organic three-phase interfacial synthesis of coral-like polypyrrole toward enhanced electrochemical capacitance

International Nuclear Information System (INIS)

Hou Linrui; Yuan Changzhou; Li Diankai; Yang Long; Shen Laifa; Zhang Fang; Zhang Xiaogang

2011-01-01

Highlights: → Interfacial synthesis strategies are proposed to synthesize PPy samples. → Water/ionic liquid /organic three-phase interface for preparing coral-like PPy. → Coral-like PPy with more ordered structure and better electronic conductivity. → Coral-like PPy owns higher rate performance and better electrochemical stability. - Abstract: Two interfacial synthesis strategies are proposed to synthesize polypyrrole samples for electrochemical capacitors (ECs). In contrast to water/organic two-phase route, unique water/ionic liquid (IL)/organic three-phase interface strategy is first performed to prepare coral-like polypyrrole with even better electrochemical capacitance, where 1-Ethyl-3-methylimidazolium tetrafluoroborate IL, as a 'buffering zone', is set between the water and organic phases to control the morphology and micro-structure of the polypyrrole phase during polymerization. The polypyrrole synthesized by three-phase interfacial route owns more ordered structure, less charge transfer resistance and better electronic conductivity, compared with two-phase method, and delivers larger specific capacitance, higher rate performance and better electrochemical stability at large current densities in 3 M KCl aqueous electrolyte.

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

International Nuclear Information System (INIS)

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

2006-01-01

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

Electrochemical synthesis of nanosized hydroxyapatite by pulsed direct current method

Energy Technology Data Exchange (ETDEWEB)

Nur, Adrian; Rahmawati, Alifah; Ilmi, Noor Izzati; Affandi, Samsudin; Widjaja, Arief [Departement of Chemical Engineering, Faculty of Industrial Technology, Sepuluh Nopember Institute of Technology, Kampus ITS Sukolilo, Surabaya 60111 (Indonesia)

2014-02-24

Synthesis of nanosized of hydroxyapatite (HA) by electrochemical pulsed direct current (PDC) method has been studied. The aim of this work is to study the influence of various PDC parameters (pH initial, electrode distance, duty cycle, frequency, and amplitude) on particle surface area of HA powders. The electrochemical synthesis was prepared in solution Ca{sup 2+}/EDTA{sup 4−}/PO{sub 4}{sup 3+} at concentration 0.25/0.25/0.15 M for 24 h. The electrochemical cell was consisted of two carbon rectangular electrodes connected to a function generator to produce PDC. There were two treatments for particles after electrosynthesized, namely without aging and aged for 2 days at 40 °C. For both cases, the particles were filtered and washed by demineralized water to eliminate the impurities and unreacted reactants. Then, the particles were dried at 100 °C for 2 days. The dried particles were characterized by X-ray diffraction, surface area analyzer, scanning electron microscopy (SEM), Fourier transform infrared spectra and thermogravimetric and differential thermal analysis. HA particles can be produced when the initial pH > 6. The aging process has significant effect on the produced HA particles. SEM images of HA particles showed that the powders consisted of agglomerates composed of fine crystallites and have morphology plate-like and sphere. The surface area of HA particles is in the range of 25 – 91 m{sup 2}/g. The largest particle surface area of HA was produced at 4 cm electrode distance, 80% cycle duty, frequency 0.1 Hz, amplitude 9 V and with aging process.

Polymer-directed synthesis of metal oxide-containing nanomaterials for electrochemical energy storage

Science.gov (United States)

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.

Microwave assisted synthesis of MnO2 on nickel foam-graphene for electrochemical capacitor

International Nuclear Information System (INIS)

Bello, A.; Fashedemi, O.O.; Fabiane, M.; Lekitima, J.N.; Ozoemena, K.I.; Manyala, N.

2013-01-01

Highlights: •Three-dimensional synthesis of graphene using CVD. •Hydrothermal deposition (microwave irradiation) of MnO 2 on graphene. •Morphologies of the composite reveals flower-like nanostructures of MnO 2 on graphene. •Composite exhibit excellent electrochemical performance. -- Abstract: A green chemistry approach (hydrothermal microwave irradiation) has been used to deposit manganese oxide on nickel foam-graphene. The 3D graphene was synthesized using nickel foam template by chemical vapor deposition (CVD) technique. Raman spectroscopy, X-ray diffraction (XRD), scanning electron and transmission electron microscopies (SEM and TEM) have been used to characterize structure and surface morphology of the composite, respectively. The Raman spectroscopy measurements on the samples reveal that 3D graphene consists of mostly few layers with low defect density. The composite was tested in a three electrode configuration for electrochemical capacitor, and exhibited a specific capacitance of 305 F g −1 at a current density of 1 A g −1 and showed excellent cycling stability. The obtained results demonstrate that microwave irradiation technique could be a promising approach to synthesis graphene based functional materials for electrochemical applications

Synthesis, Characterization, and Electrochemical Properties of Polyaniline Thin Films

Science.gov (United States)

Rami, Soukaina

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

Towards a carbon independent and CO2-free electrochemical membrane process for NH3 synthesis.

Science.gov (United States)

Kugler, K; Ohs, B; Scholz, M; Wessling, M

2014-04-07

Ammonia is exclusively synthesized by the Haber-Bosch process starting from precious carbon resources such as coal or CH4. With H2O, H2 is produced and with N2, NH3 can be synthesized at high pressures and temperatures. Regrettably, the carbon is not incorporated into NH3 but emitted as CO2. Valuable carbon sources are consumed which could be used otherwise when carbon sources become scarce. We suggest an alternative process concept using an electrochemical membrane reactor (ecMR). A complete synthesis process with N2 production and downstream product separation is presented and evaluated in a multi-scale model to quantify its energy consumption. A new micro-scale ecMR model integrates mass, species, heat and energy balances with electrochemical conversions allowing further integration into a macro-scale process flow sheet. For the anodic oxidation reaction H2O was chosen as a ubiquitous H2 source. Nitrogen was obtained by air separation which combines with protons from H2O to give NH3 using a hypothetical catalyst recently suggested from DFT calculations. The energy demand of the whole electrochemical process is up to 20% lower than the Haber-Bosch process using coal as a H2 source. In the case of natural gas, the ecMR process is not competitive under today's energy and resource conditions. In future however, the electrochemical NH3 synthesis might be the technology-of-choice when coal is easily accessible over natural gas or limited carbon sources have to be used otherwise but for the synthesis of the carbon free product NH3.

Room-temperature Electrochemical Synthesis of Carbide-derived Carbons and Related Materials

Energy Technology Data Exchange (ETDEWEB)

Gogotsi, Yury [Drexel Univ., Philadelphia, PA (United States). Nanomaterials Group. Materials Science and Engineering Dept.

2015-02-28

This project addresses room-temperature electrochemical etching as an energy-efficient route to synthesis of 3D nanoporous carbon networks and layered 2D carbons and related structures, as well as provides fundamental understanding of structure and properties of materials produced by this method. Carbide-derived-carbons (CDCs) are a growing class of nanostructured carbon materials with properties that are desirable for many applications, such as electrical energy and gas storage. The structure of these functional materials is tunable by the choice of the starting carbide precursor, synthesis method, and process parameters. Moving from high-temperature synthesis of CDCs through vacuum decomposition above 1400°C and chlorination above 400°C, our studies under the previous DOE BES support led to identification of precursor materials and processing conditions for CDC synthesis at temperatures as low as 200°C, resulting in amorphous and highly reactive porous carbons. We also investigated synthesis of monolithic CDC films from carbide films at 250-1200°C. The results of our early studies provided new insights into CDC formation, led to development of materials for capacitive energy storage, and enabled fundamental understanding of the electrolyte ions confinement in nanoporous carbons.

Cyclization of 1,2:3,4-di-O-isopropylidene-α-D-galacto-1,6-hexodialdo-1,5-pyranose acylhydrazone and semicarbazone

OpenAIRE

Martins Alho, Miriam Amelia; Baggio, Ricardo Fortunato; D'accorso, Norma Beatriz

2015-01-01

Cyclization of 1,2:3,4-di-O-isopropylidene-α-D-galacto-1,6-hexodialdo-1,5-pyranose benzoylhydrazone using acetylating mixtures led us to the corresponding (2R)- and (2S)-5- phenyl-1,3,4-oxadiazoline derivatives. The same conditions applied to the semicarbazone produced the 5-methyl-1,3,4-oxadiazoline derivative as the main compound, which is formed with acetylating mixtures even at room temperature. X-Ray analysis and NMR techniques were used to determine the stereochemistry of the new asymme...

Electrochemical Synthesis of a Microporous Conductive Polymer Based on a Metal-Organic Framework Thin Film

KAUST Repository

Lu, Chunjing; Ben, Teng; Xu, Shixian; Qiu, Shilun

2014-01-01

A new approach to preparing 3D microporous conductive polymer has been demonstrated in the electrochemical synthesis of a porous polyaniline network with the utilization of a MOF thin film supported on a conducting substrate. The prepared porous

Alternating voltage-induced electrochemical synthesis of colloidal Au nanoicosahedra

Energy Technology Data Exchange (ETDEWEB)

McCann, Kevin; Cloud, Jacqueline E.; Yang, Yongan, E-mail: yonyang@mines.edu [Colorado School of Mines, Department of Chemistry and Geochemistry (United States)

2013-11-15

A simple method of alternating voltage-induced electrochemical synthesis has been developed to synthesize highly dispersed colloidal Au nanoicosahedra of 14 ± 3 nm in size. This simple and effective method uses a common transformer to apply a zero-offset alternating voltage to a pair of identical Au electrodes that are immersed in an electrolyte solution containing ligands. The obtained Au nanoicosahedra in this work are among the smallest Au icosahedra synthesized in aqueous solutions. A series of experimental conditions have been studied, such as voltage, the electrolyte identity and concentration, stabilizer identity and concentration, and reaction temperature. The mechanistic study indicates that Au nanoicosahedra are produced on electrode surfaces through an intermediate state of AuO{sub x}. The kinetic rate constant of these Au icosahedra in catalyzing the reduction of 4-nitrophenol with sodium borohydride is found much larger than the literature values of similar Au nanocrystals. In addition, the synthesis of Au–Pd-alloyed NCs has also been attempted.Graphical Abstract.

Electrochemical Study of Bromide in the Presence of 1,3-Indandione. Application to the Electrochemical Synthesis of Bromo Derivatives of 1,3-Indandione

Directory of Open Access Journals (Sweden)

N. Akaberi

2001-06-01

Full Text Available The electrochemical oxidation of bromide in the presence of 1,3-indandione (1 in water/acetic acid and methanol/acetic acid mixtures has been studied by cyclic voltammetry and controlled-potential coulometry. The results indicate the participation of 1,3-indandione in the bromination reaction. On the basis of the electroanalytical and preparative results a reaction mechanism including electron transfer, chemical reaction and regeneration of bromide was discussed. The electrochemical synthesis of bromo derivatives of 1,3-indandione (2-3 has been successfully performed at constant current, in an undivided cell, in good yield and purity.

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

International Nuclear Information System (INIS)

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

2014-01-01

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

A New Type of Synthesis of 1,2,3-Thiadiazole and 1,2,3-Diazaphosphole Derivatives Via-Hurd-Mori Cyclization

Directory of Open Access Journals (Sweden)

Mona A. Hosny

2012-01-01

Full Text Available We present a short and efficient synthesis of the title compounds starting with cheap and readily available camphor and derivatives of acetophenone. The optimized sequence allows the large-scale preparation of this new type of synthesis in a few steps. New 1,2,3-thiadiazole and 1,2,3-diazaphosphole derivatives 11-20, were prepared from the ketones 1-5 via the corresponding semicarbazones 6-10. The Hurd-Mori and Lalezari methods were used, respectively, for the preparation of these 1,2,3-thiadiazole and 1,2,3-diazaphospholene derivatives. These derivatives exhibit anticancer effect due to their high potential biological activity.

Effect of the synthesis method on the microstructure, morphology and electrochemical characteristics of α-Fe2O3 anodes for Lithium ion batteries

International Nuclear Information System (INIS)

Uzunov, I.; Klissurski, D.; Uzunova, S.; Aleksandrova, A.

2009-01-01

Effect of the synthesis method and temperature on some structural characteristics and electrochemical behaviour was investigated for samples of α-Fe 2 O 3 prepared from different precursors. The phase composition, morphology and crystallinity of the obtained materials were determined by X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM). The electrochemical behaviour of the synthesized samples was studied within voltage range 0.01-2.5V and various current densities. The electrochemical behaviour of the obtained active anode materials was found to depend mostly on the ratio between mean particle size (MPS) and mean coherent domain size (MCDS). It was found that the ratio depends on the synthesis method and calcination temperature. By optimization of the synthesis processes α-Fe 2 O 3 was prepared with optimal microstructure and particle size, a promising anode material for lithium ion batteries. (authors)

Synthesis and electrochemical properties of peripheral carbazole functional Ter(9,9-spirobifluorene)s.

Science.gov (United States)

Tang, Shi; Liu, Meirong; Gu, Cheng; Zhao, Yang; Lu, Ping; Lu, Dan; Liu, Linlin; Shen, Fangzhong; Yang, Bing; Ma, Yuguang

2008-06-06

A facile approach for synthesis of spirobifluorene trimers with peripheral carbazole functional groups by utilizing Suzuki coupling as the key reaction has been developed. These novel compounds exhibit blue emission with high quantum yields in solution and thin films, and excellent spectral stability upon photoirradiation and annealing in air. By the introduction of carbazole groups, the oxidation potentials of spirobifluorene trimers S TCPC-6 and STCPC-4 were significantly lower than that of model compound STHPH without peripheral carbazole groups, which reflect that the title compounds process higher HOMO energy level and better hole-injection ability. Highly luminescent films were obtained by electrochemical coupling between carbazole units. Pure blue-emission single-layer LEDs based on electrochemical deposition films as light emitting layers were achieved.

Excellent electrochemical performances of cabbage-like polyaniline fabricated by template synthesis

Science.gov (United States)

Hu, Chenglong; Chen, Shaoyun; Wang, Yuan; Peng, Xianghong; Zhang, Weihong; Chen, Jian

2016-07-01

In this article, we explore a novel route to fabricate cabbage-like polyaniline (PANI) by in situ polymerization of aniline using the hydroxylated poly (methyl methacrylate) nanospheres (i.e. PMMAsbnd OHsbnd NS) as a template. A maximum specific capacitance of 584 F/g (the current density is 0.1 A/g) is achieved at 10 mV s-1 as well as a high stability of over 3000 cycles (the decrease in the SC is ∼9.1%), which suggests the potential application of the cabbage-like polyaniline in supercapacitors. The predominant electrochemical performances of the cabbage-like polyaniline can be attributed to their large surface area and larger-scale π-π conjugated system present in the quinoid structure of the PANI molecular chain, which can drastically facilitate electron diffusion and improve the utilization of the electroactive PANI during the charge/discharge processes. Accordingly, the facility of charge transfer can decrease resistance along with the PANI molecular chain to improve the electrochemical stability and achieve high-capacitance response characteristics. The present study introduces a new synthesis method for the development of various morphology of other conducting polymer, which may find potential applications in a variety of high-performance electrochemical devices.

Optimization on electrochemical synthesis of HKUST-1 as candidate catalytic material for Green diesel production

Science.gov (United States)

Lestari, W. W.; Nugraha, R. E.; Winarni, I. D.; Adreane, M.; Rahmawati, F.

2016-04-01

In the effort to support the discovery of new renewable energy sources in Indonesia, biofuel is one of promising options. The conversion of vegetable oil into ready-biofuel, especially green diesel, needs several steps, one of which is a hydrogenation or hydro-deoxygenation reaction. In this case, the catalyst plays a very important role regarding to its activity and selectivity, and Metal-Organic Frameworks (MOFs) becoming a new generation of heterogeneous catalyst in this area. In this research, a preliminary study to optimize electrochemical synthesis of the catalytic material based on MOFs, namely HKUST-1 [Cu3(BTC)2], has been conducted. Some electrochemical reaction parameters were tested, for example by modifying the electrochemical synthetic conditions, i.e. by performing variation of voltages (12, 13, 14, and 15 Volt), temperatures (RT, 40, 60, and 80 °C) and solvents (ethanol, water, methanol and dimethyl-formamide (DMF)). Material characterization was carried out by XRD, SEM, FTIR, DTA/TG and SAA. The results showed that the optimum synthetic conditions of HKUST-1 are performed at room temperature in a solvent combination of water: ethanol (1: 1) and a voltage of 15 Volt for 2 hours. The XRD-analysis revealed that the resulted peaks are identical to the simulated powder pattern generated from single crystal data and comparable to the peaks of solvothermal method. However, the porosity of the resulting material through electrochemical method is still in the range of micro-pore according to IUPAC and 50% smaller than the porosity resulted from solvothermal synthesis. The corresponding compounds are thermally stable until 300 °C according to TG/DTA.

Low Temperature Synthesis, Chemical and Electrochemical Characterization of LiNi(x)Co(1-x)O2 (0 less than x less than 1)

Science.gov (United States)

Nanjundaswamy, K. S.; Standlee, D.; Kelly, C. O.; Whiteley, R. V., Jr.

1997-01-01

A new method of synthesis for the solid solution cathode materials LiNi(x)Co(1-x)O2 (0 less than x less than 1) involving enhanced reactions at temperatures less than or equal to 700 deg. C, between metal oxy-hydroxide precursors MOOH (M = Ni, Co) and Li-salts (Li2CO3, LiOH, and LiNO3) has been investigated. The effects of synthesis conditions and sources of Li, on phase purity, microstructure, and theoretical electrochemical capacity (total M(3+) content) are characterized by powder X-ray diffraction analysis, scanning electron microscopy, chemical analysis and room temperature magnetic susceptibility. An attempt has been made to correlate the electrochemical properties with the synthesis conditions and microstructure.

Synthesis of magnetite nanoparticles using electrochemical oxidation

Directory of Open Access Journals (Sweden)

Ye. Ya. Levitin

2014-08-01

Full Text Available The monodisperse magnetite nanoparticles are promising for use in the biomedical industry for targeted drug delivery, cell separation and biochemical products, Magnetic Resonance Imaging, immunological studies, etc. Classic method for the synthesis of magnetite is the chemical condensation Elmore’s, it is simple and cheap, but it is complicated by the formation of side compounds which impair the magnetic properties of the final product. Biological and medical purposes require high purity magnetite nanoparticles. Electrochemical methods of producing nanoparticles of magnetite acquire significant spread. The kinetics of electrochemical processes are a function of a larger number of parameters than the kinetics of conventional chemical reaction, thus electrochemical reactions can be thinner and more completely adjusted to give a predetermined size nanoparticles. In the kinetics of the electrochemical oxidation and reduction the important role is played by the nature of the electrode. In many industrial processes, it is advisable to use lead dioxide anodes with titanium current lead. Purpose of the work To determine the optimum conditions of electrochemical oxidation of Fe2+ Fe3+to produce magnetite with high purity and improved magnetic characteristics. Materials and methods Electrochemical studies were carried out in a glass cell ЯСЭ-2 using a potentiostat ПИ-50-1.1 and a recording device ПДА1. Reference electrode - silver chloride ЭВЛ1М 3.1, potentials listed on the hydrogen scale. The test solution contained 80 g/ l FeSO4×7H2O and H2SO4(to pH 1. The pH of the solution was measured with a pH–meter « рН–150». Concentration ratio of Fe3+/Fe2+in the solution was measured by permanganometric method. Magnetite particle sizes were measured by an electron microscope computer ЭВМ-100Л, an increasing is 2×105. Saturation magnetization was evaluated by the magnetization curve, for the measured sample in the field with strength

Electrochemically Active Biofilms Assisted Nanomaterial Synthesis for Environmental Applications

KAUST Repository

Ahmed, Elaf

2017-12-01

Nanomaterials have a great potential for environmental applications due to their high surface areas and high reactivity. This dissertation investigated the use of electrochemically active biofilms (EABs) as a synthesis approach for the fabrication and environmental applications of different nanomaterials. Bacteria in EABs generate electrons upon consuming electron donor and have the ability to transport these electrons to solid or insoluble substrates through extracellular electron transport (EET) mechanism. The extracellularly transported electrons, once utilized, can lead to nanoparticle synthesis. In this dissertation, noble metal (i.e., Au, Pd, and Pt) ultra-small nanoparticles (USNPs) were first synthesized with the assistance by the EABs. The assynthesized USNPs had a size range between 2 and 7 nm and exhibited excellent catalytic performance in dye decomposition. Also in this research, a two-dimensional (2D) cobalt nanosheet was successfully synthesized in the presence of EABs. A simple biogenic route led to the transformation of cobalt acetate to produce a green, toxic free homogeneous 2D cobalt nanosheet structure. Further, TiO2 nanotubes were successfully combined with the noble metal USNPs to enhance their photocatalytic activity. In this work, for the first time, the noble metal USNPs were directly reduced and decorated on the internal surfaces of the TiO2 nanotubes structure assisted by the EABs. The USNPs modified TiO2 nanotubes generated significantly improved photoelectrocatatlyic performances. This dissertation shines lights on the use of EABs in ultra-small nanoparticle synthesis.

SHORT COMMUNICATION SYNTHESIS AND PRELIMINARY ...

African Journals Online (AJOL)

a

2006 Chemical Society of Ethiopia ... 1Department of Chemistry, School of Pure & Applied Sciences, The University of the South. Pacific, Post ... bonding and stereochemistry [1-3], whereas their semicarbazones analogs received much less.

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

Science.gov (United States)

Chou, Shulei; Cheng, Fangyi; Chen, Jun

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

Novel Electrochemical Synthesis of Polypyrrole/Ag Nanocomposite and Its Electrocatalytic Performance towards Hydrogen Peroxide Reduction

OpenAIRE

Ruma Gupta; Kavitha Jayachandran; J. S. Gamare; B. Rajeshwari; Santosh K. Gupta; J. V. Kamat

2015-01-01

A simple electrochemical method of synthesis of polypyrrole/silver (PPy/Ag) nanocomposite is presented. The method is based on potentiodynamic polymerization of pyrrole followed by electrodeposition of silver employing a single potentiostatic pulse. The synthesized PPy film has embedded Ag nanocubes. The morphology and structure of the resulting nanocomposite were characterized by field emission scanning electron microscopy and X-ray diffraction. Electron paramagnetic resonance studies showed...

Identification of semicarbazones, thiosemicarbazones and triazine nitriles as inhibitors of Leishmania mexicana cysteine protease CPB.

Directory of Open Access Journals (Sweden)

Jörg Schröder

Full Text Available Cysteine proteases of the papain superfamily are present in nearly all eukaryotes. They play pivotal roles in the biology of parasites and inhibition of cysteine proteases is emerging as an important strategy to combat parasitic diseases such as sleeping sickness, Chagas' disease and leishmaniasis. Homology modeling of the mature Leishmania mexicana cysteine protease CPB2.8 suggested that it differs significantly from bovine cathepsin B and thus could be a good drug target. High throughput screening of a compound library against this enzyme and bovine cathepsin B in a counter assay identified four novel inhibitors, containing the warhead-types semicarbazone, thiosemicarbazone and triazine nitrile, that can be used as leads for antiparasite drug design. Covalent docking experiments confirmed the SARs of these lead compounds in an effort to understand the structural elements required for specific inhibition of CPB2.8. This study has provided starting points for the design of selective and highly potent inhibitors of L. mexicana cysteine protease CPB that may also have useful efficacy against other important cysteine proteases.

Solvothermal synthesis of Li–Al layered double hydroxides and their electrochemical performance

International Nuclear Information System (INIS)

Wei, Jinbo; Gao, Zan; Song, Yanchao; Yang, Wanlu; Wang, Jun; Li, Zhanshuang; Mann, Tom; Zhang, Milin; Liu, Lianhe

2013-01-01

In this paper, for the first time, Li/Al layered double hydroxides (LDHs) were synthesized by a facile and environment-friendly solvothermal approach. X-ray diffraction patterns show that the as-prepared products belong to the hexagonal phase. Well-defined LDHs particles with spiral-shape (1–2 μm), hexagonal (2–3 μm) and petal-like structures (10–15 μm) have been successfully fabricated by adjusting the content of water/ethanol in the synthesis process. A possible growth mechanism was proposed for the formation of these structures. Their electrochemical performances were investigated by cyclic voltammetry, galvanostatic charge/discharge test and electrochemical impedance spectroscopy. The hexagonal Li/Al LDHs calcined at 450 °C exhibit the specific capacitance of 848 F g −1 at a current density of 1.25 A g −1 . The high specific capacitance and remarkable rate capacity of Li/Al LDHs are promising for applications in capacitors and low-cost aqueous lithium ion batteries. - Graphical abstract: Hexagonal Li/Al layered double hydroxides (LDHs) with high specific surface area and remarkable rate capacity via a facile and environmentally friendly solvothermal approach. Highlights: ► Li/Al LDHs with different morphologies were fabricated by a solvothermal method. ► Hexagonal Li/Al LDHs display better electrochemical performance. ► A possible growth mechanism to explain the different morphology is proposed

One pot electrochemical synthesis of polymer/CNT/metal nanoparticles for fuel cell applications

Science.gov (United States)

Ventrapragada, Lakshman; Zhu, Jingyi; Karakaya, Mehmet; Podila, Ramakrishna; Rao, Apparao; Clemson Nanomaterials center Team

Carbon nanotubes (CNTs) have become a key player in the design of materials for energy applications. They gained their popularity in industrial and scientific research due to their unique properties like excellent conductivity, high surface area, etc. Here we used chemical vapor deposition (CVD) to synthesize two types of CNTs namely, helically coiled CNTs and vertically aligned CNTs. These CNTs were subsequently used to make composites with conducting polymers and metal nanoparticles. One pot electrochemical synthesis was designed to electropolymerize aniline, pyrrole etc. on the surface of the electrode with simultaneous deposition of platinum and gold metal nanoparticles, and CNTs in the polymer matrix. The as synthesized composite materials were characterized with scanning electron microscope for surface morphology and spectroscopic techniques like Raman, UV-Vis for functionality. These were used to study electrocatalytic oxidation of methanol and ethanol for alkaline fuel cell applications. Electrodes fabricated from these composites not only showed good kinetics but also exhibited excellent stability. Uniqueness of this composite lies in its simple two step synthesis and it doesn't involve any surfactants unlike conventional chemical synthesis routes.

Synthesis and electrochemical properties of binary MgTi and ternary MgTiX (X=Ni, Si) hydrogen storage alloys

NARCIS (Netherlands)

Gobichettipalayam Manivasagam, T.; Iliksu, M.; Danilov, D.L.; Notten, P.H.L.

2017-01-01

Mg-based hydrogen storage alloys are promising candidate for many hydrogen storage applications because of the high gravimetric hydrogen storage capacity and favourable (de)hydrogenation kinetics. In the present study we have investigated the synthesis and electrochemical hydrogen storage properties

Electrochemical Processes

DEFF Research Database (Denmark)

Bech-Nielsen, Gregers

1997-01-01

The notes describe in detail primary and secondary galvanic cells, fuel cells, electrochemical synthesis and electroplating processes, corrosion: measurments, inhibitors, cathodic and anodic protection, details of metal dissolution reactions, Pourbaix diagrams and purification of waste water from...

Electrodeposition synthesis and electrochemical properties of nanostructured {gamma}-MnO{sub 2} films

Energy Technology Data Exchange (ETDEWEB)

Chou, Shulei; Cheng, Fangyi; Chen, Jun [Institute of New Energy Material Chemistry, Nankai University, Tianjin 300071 (China)

2006-11-08

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

Synthesis, characterization and electrochemical properties of 4.8 V LiNi{sub 0.5}Mn{sub 1.5}O{sub 4} cathode material in lithium-ion batteries

Energy Technology Data Exchange (ETDEWEB)

Chi, Le Ha [Faculty of Engineering Physics and NanoTechnology, College of Technology, 144 Xuan Thuy Road, Hanoi (Viet Nam)] [Vietnamese Academy of Science and Technology, 18 Hoang Quoc Viet Street, Cau Giay District, Hanoi (Viet Nam); Dinh, Nguyen Nang [Faculty of Engineering Physics and NanoTechnology, College of Technology, 144 Xuan Thuy Road, Hanoi (Viet Nam); Brutti, Sergio, E-mail: sergio.brutti@uniroma1.i [Department of Chemistry, University of Rome ' La Sapienza' , P.le Aldo Moro 5, 00185 Rome (Italy); Scrosati, Bruno [Department of Chemistry, University of Rome ' La Sapienza' , P.le Aldo Moro 5, 00185 Rome (Italy)

2010-07-15

In this work the synthesis of a nickel doped cubic manganese spinel has been studied for application as cathode material in secondary lithium batteries. Six different experimental approaches have been tested in order to carry out a screening of the various possible synthetic routes. The used synthetic strategies were wet chemistry (WC), solid state (SS), combustion synthesis (CS), cellulose-based sol-gel synthesis (SG-C), ascorbic acid-based sol-gel synthesis (SG-AA) and resorcinol/formaldehyde-based sol-gel synthesis (SG-RF). The goal of our study is to obtain insights about how the synthesis conditions can be modified in order to achieve a material with improved electrochemical performances in such devices, especially in high current operating regimes. The synthesized materials have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS), atomic absorption, inductively coupled plasma (ICP-MS) atomic emission spectroscopy, surface area measurements and tested as high voltage cathodes in Li-ion electrochemical devices.

One-step electrochemical synthesis and photoelectric conversion of a ZnO/Se/RGO composite

International Nuclear Information System (INIS)

Wang, Lei; Zhang, Chunyan; Zhang, Shengyi; Niu, Helin; Song, Jiming; Mao, Changjie; Jin, Baokang; Tian, Yupeng

2015-01-01

Using Zn(NO 3 ) 2 , H 2 SeO 3 and graphene oxide as precursors, the zinc oxide/selenium/reduced graphene oxide (ZnO/Se/RGO) composite was facilely electrodeposited on the surface of indium tin oxide glass. The conditions for electrochemical synthesis such as electrodeposition potential and electrolyte composition were studied. The morphology and crystallization of the products as-prepared were characterized using scanning electron microscopy (SEM) and x-ray diffractometry (XRD) respectively. The light absorption and conductivity of the products were studied by UV-visible spectroscopy (UV-vis) and electrochemical impedance spectroscopy (EIS). Based on a series of experimental results, the photoelectrical conversion mechanism and effect factors of the products were explored. By means of synergistic action of n-type ZnO, p-type Se and conductive RGO, the ZnO/Se/RGO composite showed excellent photoelectric conversion under visible light irradiation. (paper)

Recent progress in layered double hydroxide based materials for electrochemical capacitors: design, synthesis and performance.

Science.gov (United States)

Zhao, Mingming; Zhao, Qunxing; Li, Bing; Xue, Huaiguo; Pang, Huan; Chen, Changyun

2017-10-19

As representative two-dimensional (2D) materials, layered double hydroxides (LDHs) have received increasing attention in electrochemical energy storage and conversion because of the facile tunability between their composition and morphology. The high dispersion of active species in layered arrays, the simple exfoliation into monolayer nanosheets and chemical modification offer the LDHs an opportunity as active electrode materials in electrochemical capacitors (ECs). LDHs are favourable in providing large specific surface areas, good transport features as well as attractive physicochemical properties. In this review, our purpose is to provide a detailed summary of recent developments in the synthesis and electrochemical performance of the LDHs. Their composites with carbon (carbon quantum dots, carbon black, carbon nanotubes/nanofibers, graphene/graphene oxides), metals (nickel, platinum, silver), metal oxides (TiO 2 , Co 3 O 4 , CuO, MnO 2 , Fe 3 O 4 ), metal sulfides/phosphides (CoS, NiCo 2 S 4 , NiP), MOFs (MOF derivatives) and polymers (PEDOT:PSS, PPy (polypyrrole), P(NIPAM-co-SPMA) and PET) are also discussed in this review. The relationship between structures and electrochemical properties as well as the associated charge-storage mechanisms is discussed. Moreover, challenges and prospects of the LDHs for high-performance ECs are presented. This review sheds light on the sustainable development of ECs with LDH based electrode materials.

Chemical and Electrochemical Synthesis of Polypyrrole Using Carrageenan as a Dopant: Polypyrrole/Multi-Walled Carbon Nanotube Nanocomposites

Directory of Open Access Journals (Sweden)

Mostafizur Rahaman

2018-06-01

Full Text Available In this article, iota-carrageenan (IC and kappa-carrageenan (KC are used as dopants for the chemical and electrochemical synthesis of polypyrrole (PPy. The composites of chemically synthesized PPy with multi-walled carbon nanotubes (MWNTs were prepared using an in situ technique. Both the dialyzed and non-dialyzed IC and KC were used as dopants for electrochemical polymerization of pyrrole. Chemically synthesized PPy and PPy/MWNTs composites were studied by ultraviolet visible (UV-vis absorption spectra to investigate the effect of the concentration and the incorporation of MWNTs. In addition, the electrical, thermal, mechanical, and microscopic characterizations of these films were performed to examine the effect of the dopants and MWNTs on these properties, along with their surface morphology. The films of electrochemically polymerized PPy were characterized using UV-vis absorption spectra, scanning electron microscopy, and cyclic voltammetry (CV. The results were then compared with the chemical polymerized PPy.

Synthesis and characterization of a nanocomposite of goethite nanorods and reduced graphene oxide for electrochemical capacitors

International Nuclear Information System (INIS)

Shou Qingliang; Cheng Jipeng; Zhang Li; Nelson, Bradley J.; Zhang Xiaobin

2012-01-01

We report a one-step synthesis of a nanocomposite of goethite (α-FeOOH) nanorods and reduced graphene oxide (RGO) using a solution method in which ferrous cations serve as a reducing agent of graphite oxide (GO) to graphene and a precursor to grow goethite nanorods. As-prepared goethite nanorods have an average length of 200 nm and a diameter of 30 nm and are densely attached on both sides of the RGO sheets. The electrochemical properties of the nanocomposite were characterized by cyclic voltammetry (CV) and chronopotentiometry (CP) charge–discharge tests. The results showed that goethite/RGO composites have a high electrochemical capacitance of 165.5 F g −1 with an excellent recycling capability making the material promising for electrochemical capacitors. - Graphical abstract: The reduced graphene oxide sheets are decorated with goethite nanorods. The as-prepared composite exhibits a high electrochemical capacitance with good recycling capability, which is promising for supercapacitor applications. Higlights: ► Ferrous ions act as reductant of graphite oxide and precursor of goethite nanorods. ► Goethite nanorods are attached on both sides of the reduced graphene oxide sheets. ► Composite exhibits a high specific capacitance and a good recycling capability. ► Composite is promising for supercapacitor applications.

A Simple Synthesis of Two-Dimensional Ultrathin Nickel Cobaltite Nanosheets for Electrochemical Lithium Storage

International Nuclear Information System (INIS)

Zhu, Youqi; Cao, Chuanbao

2015-01-01

We report a simple microwave-assisted method to fabricate high-quality two-dimensional (2D) ultrathin NiCo 2 O 4 nanosheets with a geometrically graphene-like architecture. The unique large-area nanostructures represent an ultrahigh surface atomic ratio with almost all active elements exposed outside for surface-dependent electrochemical reaction processes. Experimental results reveal that the as-synthesized ultrathin NiCo 2 O 4 nanosheets show excellent electrochemical performances for lithium storage application. The ultrathin NiCo 2 O 4 nanosheets could deliver a high first discharge capacity (1287.1 mAh g −1 ) with initial Coulombic efficiency of 80.0% at 200 mA g −1 current density. The reversible lithium storage capacity still retains at 804.8 mAh g −1 in the 100th cycle, suggesting a good cycling stability. The excellent electrochemical properties of the as-synthesized NiCo 2 O 4 nanosheets could be ascribed to the unique ultrathin 2D architecture, which could offer large exposed active surface with more lithium-insertion channels and significantly reduce lithium ion diffusion distance. The cost-efficient synthesis and excellent lithium storage properties make the 2D NiCo 2 O 4 nanosheets as a promising anode material for high-performance lithium ion batteries

Electrochemical synthesis of polypyrrole on ferrous and non-ferrous metals from sweet aqueous electrolytic medium

International Nuclear Information System (INIS)

Bazzaoui, M.; Martins, J.I.; Reis, T.C.; Bazzaoui, E.A.; Nunes, M.C.; Martins, L.

2005-01-01

The electrodeposition of polypyrrole (PPy) on oxidizable metals such as aluminum and iron has been achieved in aqueous medium of saccharin and pyrrole. Scanning electron microscopy and X-ray photoelectron spectroscopy analysis reveal a good homogeneity of the obtained PPy film. The electrochemical synthesis of PPy coating has been achieved successfully under potentiodynamic, galvanostatic and potentiostatic techniques. The corrosion experiments performed in HCl show that the PPy coating increases the corrosion potential and decreases the corrosion current density

Electrochemical synthesis of 1D core-shell Si/TiO2 nanotubes for lithium ion batteries

Science.gov (United States)

Kowalski, Damian; Mallet, Jeremy; Thomas, Shibin; Nemaga, Abirdu Woreka; Michel, Jean; Guery, Claude; Molinari, Michael; Morcrette, Mathieu

2017-09-01

Silicon negative electrode for lithium ion battery was designed in the form of self-organized 1D core-shell nanotubes to overcome shortcomings linked to silicon volume expansion upon lithiation/delithiation typically occurring with Si nanoparticles. The negative electrode was formed on TiO2 nanotubes in two step electrochemical synthesis by means of anodizing of titanium and electrodeposition of silicon using ionic liquid electrolytes. Remarkably, it was found that the silicon grows perpendicularly to the z-axis of nanotube and therefore its thickness can be precisely controlled by the charge passed in the electrochemical protocol. Deposited silicon creates a continuous Si network on TiO2 nanotubes without grain boundaries and particle-particle interfaces, defining its electrochemical characteristics under battery testing. In the core-shell system the titania nanotube play a role of volume expansion stabilizer framework holding the nanostructured silicon upon lithiation/delithiation. The nature of Si shell and presence of titania core determine stable performance as negative electrode tested in half cell of CR2032 coin cell battery.

One pot synthesis of dandelion-like polyaniline coated gold nanoparticles composites for electrochemical sensing applications.

Science.gov (United States)

Lu, Zhiwei; Dai, Wanlin; Liu, Baichen; Mo, Guangquan; Zhang, Junjun; Ye, Jiaping; Ye, Jianshan

2018-04-18

In this work, we report a facile and green strategy for one pot and in-situ synthesis of a dandelion-like conductive polyaniline coated gold nanoparticle nanocomposites (Au@PANI). The Au@PANI was characterized by SEM, TEM, XRD, TGA, FTIR, UV-vis and conductivity measurement, respectively. Newly-designed Au@PANI materials possessed a significantly high conductivity and strong adsorption capability. Thus, the Au@PANI modified glassy carbon electrode (GCE) was utilized for construct a novel electrochemical sensor for the simultaneous assay of Pb 2+ and Cu 2+ using square wave anodic stripping voltammetry (SWASV). Under the optimized conditions, an excellent electrochemical response in the simultaneous of Pb 2+ and Cu 2+ with detection limit of 0.003 and 0.008 μM (S/N = 3), respectively. Moreover, the prepared sensors realized an excellent reproducibility, repeatability and long term stability, as well as reliable practical assays in real water samples. Besides, the possible formation mechanism and sensing mechanism of Au@PANI nanocomposites have been discussed in detail. We believe this study provides a novel method of fabrication of noble metal nanoparticles decorated conducting polymer materials for the electrochemical sensing applications. Copyright © 2018 Elsevier Inc. All rights reserved.

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-06-15

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

Characterization and electrochemical performances of MoO2 modified LiFePO4/C cathode materials synthesized by in situ synthesis method

International Nuclear Information System (INIS)

He, Jichuan; Wang, Haibin; Gu, Chunlei; Liu, Shuxin

2014-01-01

Graphical abstract: The MoO 2 modified LiFePO 4 /C cathode materials were synthesized by in situ synthesis method. MoO 2 can sufficiently coat on the LiFePO 4 /C particles surface and does not alter LiFePO 4 crystal structure, and the adding of MoO 2 decreases the particles size and increases the tap density of cathode materials. The existence of MoO 2 improves electrochemical performance of LiFePO 4 cathode materials in specific capability and lithium ion diffusion and charge transfer resistance of cathode materials. - Highlights: • The MoO 2 modified LiFePO 4 /C cathode materials were synthesized by in situ synthesis method. • The existence of MoO 2 decreases the particles size and increases the tap density of cathode materials. • MoO 2 can sufficiently coat on the surface of LiFePO 4 /C cathode materials. • The existence of MoO 2 enhanced electrochemical performance of LiFePO 4 /C cathode materials. - Abstract: The MoO 2 modified LiFePO 4 /C cathode materials were synthesized by in situ synthesis method. Phase compositions and microstructures of the products were characterized by X-ray powder diffraction (XRD), SEM, TEM and EDS. Results indicate that MoO 2 can sufficiently coat on the LiFePO 4 surface and does not alter LiFePO 4 crystal structure, the existence of MoO 2 decreases the particles size and increases the tap density of cathode materials. The electrochemical behavior of cathode materials was analyzed using galvanostatic measurement, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The results show that the existence of MoO 2 improves electrochemical performance of LiFePO 4 cathode materials in specific capability and lithium ion diffusion and charge transfer resistance. The initial charge–discharge specific capacity and apparent lithium ion diffusion coefficient increase, the charge transfer resistance decreases with MoO 2 content and maximizes around the MoO 2 content is 5 wt%. It has been had further proved that

Electrochemical polymer electrolyte membranes

CERN Document Server

Fang, Jianhua; Wilkinson, David P

2015-01-01

Electrochemical Polymer Electrolyte Membranes covers PEMs from fundamentals to applications, describing their structure, properties, characterization, synthesis, and use in electrochemical energy storage and solar energy conversion technologies. Featuring chapters authored by leading experts from academia and industry, this authoritative text: Discusses cutting-edge methodologies in PEM material selection and fabricationPoints out important challenges in developing PEMs and recommends mitigation strategies to improve PEM performanceAnalyzes the cur

Synthesis, characterisation and electrochemical evaluation of reduced graphene oxide modified antimony nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Silwana, Bongiwe; Horst, Charlton van der [Natural Resources and the Environment (NRE), Council for Scientific and Industrial Research (CSIR), Stellenbosch 7600 (South Africa); SensorLab, Department of Chemistry, University of the Western Cape, Bellville 7535 (South Africa); Iwuoha, Emmanuel [SensorLab, Department of Chemistry, University of the Western Cape, Bellville 7535 (South Africa); Somerset, Vernon, E-mail: vsomerset@csir.co.za [Natural Resources and the Environment (NRE), Council for Scientific and Industrial Research (CSIR), Stellenbosch 7600 (South Africa)

2015-10-01

This paper demonstrates some aspects on the synthesis and characterisation of nanoparticles of metallic alloys using polyvinyl alcohol as a stabiliser, which combines high surface area and superior hybrid properties. The present experimental design was to synthesise a nanocomposite of reduced graphene oxide and antimony nanoparticles to be used as thin films for macro- and micro-carbon electrodes for enhancing sensing of different toxic metal pollutants in the environment. The synthetic process of reduced graphene oxide was done using the modified Hummers method while antimony pentachloride was reduced with sodium borohydride into nanoparticles of antimony using polyvinyl-alcohol as a stabiliser. The systematic investigation of morphology was done by scanning electron microscopy and high resolution-transmission electron microscope, which revealed the synthesis of a product, consists of reduced graphene oxide antimony nanoparticles. The electrochemical behaviour of the reduced graphene oxide antimony nanoparticles coated on a glassy carbon electrode was performed using voltammetric and impedance techniques. Electrochemical impedance measurements showed that the overall resistance, including the charge–transfer resistance, was smaller with reduced graphene oxide antimony nanoparticles than reduced graphene oxide and antimony nanoparticles, on their own. Evaluation of the reduced graphene oxide antimony nanoparticle sensor in the stripping voltammetry has shown a linear working range for concentration of platinum (II) between 6.0 × 10{sup −6}–5.4 × 10{sup −5} μg L{sup −1} with limit of detection of 6 × 10{sup −6} μg L{sup −1} (signal-to-noise ratio = 3), which is below the World Health Organisation guidelines for freshwater. - Highlights: • Reduced graphene oxide modified antimony nanoparticles were chemically synthesised. • TEM results show rGO-Sb nanoparticles with a diameter range of between 2 and 20 nm. • Impedance results confirm

Synthesis and Electrochemical Performance of LixMn2-yCoyO4-dCld Cathode Material

Science.gov (United States)

2016-06-13

Synthesis and Electrochemical Performance of LixMn2-yCoyO4-dCld Cathode Material Terrill B. Atwater, Paula C. Latorre, and Ashley L. Ruth U.S...low toxicity, comparable capacity, and low cost. However, this spinel suffers from capacity fading due to fracturing of the cell structure...dopants of interest include compounds containing Group VIII Row 4 (Fe, Co, and Ni) elements, cobalt in particular. In addition to fabrication method

Electrochemical synthesis and characterization of stable colloidal suspension of graphene using two-electrode cell system

Energy Technology Data Exchange (ETDEWEB)

Danial, Wan Hazman, E-mail: hazmandanial@gmail.com; Majid, Zaiton Abdul, E-mail: zaiton@kimia.fs.utm.my; Aziz, Madzlan [Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia (UTM), 81310 Skudai, Johor (Malaysia); Chutia, Arunabhiram [Institute of Fluid Sciences, Tohoku University, Sendai 980-8577 (Japan); Sahnoun, Riadh [Ibnu Sina Institute for Fundamental Science Studies, Universiti Teknologi Malaysia (UTM), 81310 Skudai, Johor (Malaysia)

2015-07-22

The present work reports the synthesis and characterization of graphene via electrochemical exfoliation of graphite rod using two-electrode system assisted by Sodium Dodecyl Sulphate (SDS) as a surfactant. The electrochemical process was carried out with sequence of intercalation of SDS onto the graphite anode followed by exfoliation of the SDS-intercalated graphite electrode when the anode was treated as cathode. The effect of intercalation potential from 5 V to 9 V and concentration of the SDS surfactant of 0.1 M and 0.01 M were investigated. UV-vis Spectroscopic analysis indicated an increase in the graphene production with higher intercalation potential. Transmission Electron Microscopy (TEM) analysis showed a well-ordered hexagonal lattice of graphene image and indicated an angle of 60° between two zigzag directions within the honeycomb crystal lattice. Raman spectroscopy analysis shows the graphitic information effects after the exfoliation process.

Lithium-deficient Li YMn2O4 spinels (0.9 ≤ Y < 1): Lithium content, synthesis temperature, thermal behaviour and electrochemical properties

International Nuclear Information System (INIS)

Pascual, Laura; Perez-Revenga, M. Luz; Rojas, Rosa M.; Rojo, Jose M.; Amarilla, J. Manuel

2006-01-01

Lithium-deficient Li Y Mn 2 O 4 spinels (LD-Li Y Mn 2 O 4 ) with nominal composition (0.9 ≤ Y 2 O 3 and LiNO 3 at temperatures ranging from 700 deg. C to 850 deg. C. X-ray diffraction data show that LD-Li Y Mn 2 O 4 spinels are obtained as single phases in the range Y = 0.975-1 at 700 deg. C and 750 deg. C. Morphological characterization by transmission electron microscopy shows that the particle size of LD-Li Y Mn 2 O 4 spinels increases on decreasing the Li-content. The influence of the Li-content and the synthesis temperature on the thermal and electrochemical behaviours has been systematically studied. Thermal analysis studies indicate that the temperature of the first thermal effect in the differential thermal analysis (DTA)/thermogravimetric (TG) curves, T C1 , linearly increases on decreasing the Li-content. The electrochemical properties of LD-Li Y Mn 2 O 4 spinels, determined by galvanostatic cycling, notably change with the synthesis conditions. So, the first discharge capacity, Q disch. , at C rate increases on rising the Li-content and the synthesis temperature. The sample Li 0.975 Mn 2 O 4 synthesized at 700 deg. C has a Q disch. = 123 mAh g -1 and a capacity retention of 99.77% per cycle. This LD-Li Y Mn 2 O 4 sample had the best electrochemical characteristics of the series

Synthesis of Pt nanoparticles on electrochemically reduced graphene oxide by potentiostatic and alternate current methods

International Nuclear Information System (INIS)

Molina, J.; Fernández, J.; Río, A.I. del; Bonastre, J.; Cases, F.

2014-01-01

Reduced graphene oxide (RGO) has been synthesized on Pt wires by means of a potentiodynamic method between + 0.6 V and − 1.4 V for 20 scans. Cyclic voltammetry characterization of the coatings showed the typical capacitative behavior of graphene. Pt nanoparticles were synthesized on Pt–RGO electrodes by means of potentiostatic methods and a comparison between different synthesis potentials (− 0.16, 0, + 0.2 and + 0.4 V) for the same synthesis charge (mC·cm −2 ) was established. The electrodes obtained were characterized in 0.5 M H 2 SO 4 solution to observe the characteristic oxidation and reduction processes of the Pt surface. A 0.5 M H 2 SO 4 /0.5 M CH 3 OH solution was used to measure the catalytic properties of the deposits against methanol oxidation. The most appropriate potential to perform the synthesis was 0 V followed by − 0.16 V and + 0.2 V. The morphology of the coatings varied depending on the potential applied as observed by scanning electron microscopy. Alternate current methods were also used to synthesize Pt nanoparticles and compare the results with the traditional potentiostatic method. Different frequencies were used: 0.1, 1, 10, 100, 1000 and 10 000 Hz. Alternate current synthesis is more efficient than traditional potentiostatic methods, obtaining more electroactive coatings with less effective synthesis time. - Highlights: • Reduced graphene oxide has been obtained by electrochemical reduction on Pt wires. • Pt nanoparticles have been obtained potentiostatically at different potentials. • Pt nanoparticles have been obtained by ac methods with different frequencies. • ac synthesis is a better synthesis method than potentiostatic synthesis

Synthesis, photophysical and electrochemical properties of water–soluble phthalocyanines bearing 8-hydroxyquinoline-5-sulfonicacid derivatives

Energy Technology Data Exchange (ETDEWEB)

Günsel, Armağan; Kocabaş, Sibel; Bilgiçli, Ahmet T. [Department of Chemistry, Sakarya University, 54140 Esentepe, Sakarya (Turkey); Güney, Sevgi [Department of Chemistry, Istanbul Technical University, 34469 Maslak, Istanbul (Turkey); Kandaz, Mehmet, E-mail: mkandaz@sakarya.edu.tr [Department of Chemistry, Sakarya University, 54140 Esentepe, Sakarya (Turkey)

2016-08-15

We have presented in this paper, the synthesis, characterization, photophysical properties and electrochemical characterization of water soluble phthalocyanines (Pcs) bearing 8-hydroxyquinoline-5-sulfonicacid conjugates and their cationic quaternized counterpart that play important roles their application in photodynamic therapy (PDT). The periphery and non-periphery substituted phthalocyanines show high solubility and low aggregation tendency due to bulky 8-hydroxyquinoline-5-sulfonicacid steric hindrance moieties and axially bound counter chlorine anion. Singlet oxygen quantum yields, photodegradation quantum yields, photophysical properties and also the nature of the substituent and solvent effect on the photophysical and photochemical parameters of α-ZnPc and β-ZnPc are reported. In electrovalent cobalt (II) and manganese (III) compounds, metal based electron transfer reactions have been observed in addition to the common phthalocyanine ring-based electron transfer processes. The effect of point of substitution on the electrochemical properties of newly synthesized phthalocyanines substituted with 8-hydroxyquinoline-5-sulfonicacid group were evaluated.

Bio-electrochemical synthesis of commodity chemicals by autotrophic acetogens utilizing CO2 for environmental remediation.

Science.gov (United States)

Jabeen, Gugan; Farooq, Robina

2016-09-01

Bio-electrochemical synthesis (BES) is a technique in which electro-autotrophic bacteria such as Clostridium ljungdahlii utilize electric currents as an electron source from the cathode to reduce CO2 to extracellular, multicarbon, exquisite products through autotrophic conversion. The BES of volatile fatty acids and alcohols directly from CO2 is a sustainable alternative for non-renewable, petroleum-based polymer production. This conversion of CO2 implies reduction of greenhouse gas emissions. The synthesis of heptanoic acid, heptanol, hexanoic acid and hexanol, for the first time, by Clostridium ljungdahlii was a remarkable achievement of BES. In our study, these microorganisms were cultivated on the cathode of a bio-electrochemical cell at -400 mV by a DC power supply at 37 degree Centrigrade, pH 6.8, and was studied for both batch and continuous systems. Pre-enrichment of bio-cathode enhanced the electroactivity of cells and resulted in maximizing extracellular products in less time. The main aim of the research was to investigate the impact of low-cost substrate CO2, and the longer cathode recovery range was due to bacterial reduction of CO2 to multicarbon chemical commodities with electrons driven from the cathode. Reactor design was simplified for cost-effectiveness and to enhance energy efficiencies. The Columbic recovery of ethanoic acid, ethanol, ethyl butyrate, hexanoic acid, heptanoic acid and hexanol being in excess of 80 percent proved that BES was a remarkable technology.

Electrochemical synthesis of magnetic nanostructures using anodic aluminum oxide templates

Science.gov (United States)

Gong, Jie

In this dissertation, template electrodeposition was employed to fabricate high quality magnetic nanostructures suited for the reliable investigation of novel spintronics phenomena such as CIMS, BMR, and CPP-GMR. Several critical aspects/steps relating to the synthesis process were investigated in this work. In order to obtain high quality magnetic nanostructures, free-standing and Si-supported anodic aluminum oxide templates with closely controlled pore diameters, lengths, as well as constriction sizes, were synthesized by anodization, followed by appropriate post-processing. The pore opening size on the barrier layer can be controlled down to 5 nm by ion beam etching. After optimization of the compositional, structural, and magnetic properties of homogeneous FeCoNiCu layers electrodeposited under different conditions, the pulsed deposition process of FeCoNI/Cu multilayers on n-Si was studied. The influence of Cu deposition potential and Fe2+ concentration on microstructure, chemical and electrochemical properties, magnetic properties, and hence magnetotransport properties were assessed. The dissolution of the FM layer during potential transition was minimized in order to control interface sharpness. Combined with the systematic sublayer thickness and FM layer composition optimization, unprecedented GMR sensitivity of 0.11%/Oe at 5-15 Oe was obtained. Growth of multilayer nanowires was performed, and contact to a single wire was attempted using an electrochemical technique. We succeeded in addressing a small number of nanowires and measured a CPP-GMR of 17%. Template electrodeposition thus provides a promising way to repeatably fabricate prototypes for spin dependent transport studies.

Synthesis and electrochemical characterization of nano-sized Ag_4Sn particles as anode material for lithium-ion batteries

International Nuclear Information System (INIS)

Schmuelling, Guido; Oehl, Nikolas; Fromm, Olga; Knipper, Martin; Kolny-Olesiak, Joanna; Plaggenborg, Thorsten; Parisi, Jürgen; Winter, Martin; Placke, Tobias

2016-01-01

For the first time, sub 10 nm sized intermetallic Ag_4Sn particles are prepared via an aqueous synthesis route in order to improve the electrochemical performance of pure Sn nanoparticles. High-resolution transmission electron microscopy, X-ray diffraction and thermogravimetric analysis are used to investigate the morphology, crystal structure and particle surface of the as prepared Ag_4Sn nanoparticles. In addition, galvanostatic cycling and cyclic voltammetry measurements are carried out to characterize the electrochemical behavior of the particles. Upon lithiation and de-lithiation a phase transformation from Ag_4Sn to Ag_3Sn is observed, which has not been reported so far. The intermetallic nanoparticle-based anode delivers a specific de-lithiation capacity of 460 mAhg"−"1 for more than 150 cycles.

Effects of size reduction on the structure and magnetic properties of core-shell Ni3Si/silica nanoparticles prepared by electrochemical synthesis

Czech Academy of Sciences Publication Activity Database

Pigozzi, G.; Mukherji, D.; Elerman, Y.; Strunz, Pavel; Gilles, R.; Hoelzel, M.; Barbier, B.; Schmutz, P.

2014-01-01

Roč. 584, JAN (2014), s. 119-127 ISSN 0925-8388 Institutional support: RVO:61389005 Keywords : intermetallics * nanostructured materials * transition metal alloys and compounds * electrochemical synthesis * crystal structure * magnetic measurements Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.999, year: 2014

Electrochemical Synthesis of a Microporous Conductive Polymer Based on a Metal-Organic Framework Thin Film

KAUST Repository

Lu, Chunjing

2014-05-22

A new approach to preparing 3D microporous conductive polymer has been demonstrated in the electrochemical synthesis of a porous polyaniline network with the utilization of a MOF thin film supported on a conducting substrate. The prepared porous polyaniline with well-defined uniform micropores of 0.84 nm exhibits a high BET surface area of 986 m2 g−1 and a high electric conductivity of 0.125 S cm−1 when doped with I2, which is superior to existing porous conducting materials of porous MOFs, CMPs, and COFs.

Study of the aqueous synthesis, optical and electrochemical characterization of alloyed Zn{sub x}Cd{sub 1-x}Te nanocrystals

Energy Technology Data Exchange (ETDEWEB)

Matos, Charlene Regina Santos [Postgraduate Program in Materials Science and Engineering, Federal University of Sergipe, São Cristóvão, SE (Brazil); Candido, Luan P.M.; Souza, Helio Oliveira [Department of Chemistry, Federal University of Sergipe, São Cristóvão, SE (Brazil); Pereira da Costa, Luiz [Institute of Technology and Research (ITP), Tiradentes University, Aracaju, SE (Brazil); Sussuchi, Eliana Midori [Department of Chemistry, Federal University of Sergipe, São Cristóvão, SE (Brazil); Gimenez, Iara F., E-mail: gimenez@ufs.br [Postgraduate Program in Materials Science and Engineering, Federal University of Sergipe, São Cristóvão, SE (Brazil); Department of Chemistry, Federal University of Sergipe, São Cristóvão, SE (Brazil); Postgraduate Program in Chemistry, Federal University of Sergipe, São Cristóvão, SE (Brazil)

2016-08-01

The effects of experimental factors such as initial reaction pH, capping ligand, and heating method on the optical and electrochemical properties of aqueous alloyed Zn{sub x}Cd{sub 1-x}Te nanocrystals were evaluated. Here the type of capping ligand (glutathione GSH and 3-mercaptopropionic acid MPA) was found to be the most significant factor in controlling the range of photoluminescence emission. Also a pronounced pH effect on the emission wavelength has been verified in the presence of GSH, in contrast to MPA for which only a minor pH effect was observed. The heating method (microwave or hydrothermal) was found to be irrelevant for the emission wavelength at the conditions studied. The electrochemical characterization in aqueous medium (cyclic voltammetry and differential pulse voltammetry) evidenced a good correlation between electrochemical and optical band gap values and allowed estimation of band edge positions. - Highlights: • ZnCdTe quantum dots were obtained by aqueous synthesis. • Nature of capping ligand was the most relevant factor. • Optical and electrochemical band gaps were well correlated.

Synthesis of graphene platelets by chemical and electrochemical route

Energy Technology Data Exchange (ETDEWEB)

Ramachandran, Rajendran; Felix, Sathiyanathan [Centre for Nanotechnology Research, VIT University, Vellore 632014, Tamil Nadu (India); Joshi, Girish M. [Materials Physics Division, School of Advanced Sciences, VIT University, Vellore 632014, Tamil Nadu (India); Raghupathy, Bala P.C., E-mail: balapraveen2000@yahoo.com [Centre for Nanotechnology Research, VIT University, Vellore 632014, Tamil Nadu (India); Research and Advanced Engineering Division (Materials), Renault Nissan Technology and Business Center India (P) Ltd., Chennai, Tamil Nadu (India); Jeong, Soon Kwan, E-mail: jeongsk@kier.re.kr [Climate Change Technology Research Division, Korea Institute of Energy Research, Yuseong-gu, Daejeon 305-343 (Korea, Republic of); Grace, Andrews Nirmala, E-mail: anirmalagrace@vit.ac.in [Centre for Nanotechnology Research, VIT University, Vellore 632014, Tamil Nadu (India); Climate Change Technology Research Division, Korea Institute of Energy Research, Yuseong-gu, Daejeon 305-343 (Korea, Republic of)

2013-10-15

Graphical abstract: A schematic showing the overall reduction process of graphite to reduced graphene platelets by chemical and electrochemical route. - Highlights: • Graphene was prepared by diverse routes viz. chemical and electrochemical methods. • NaBH{sub 4} was effective for removing oxygen functional groups from graphene oxide. • Sodium borohydride reduced graphene oxide (SRGO) showed high specific capacitance. • Electrochemical rendered a cheap route for production of graphene in powder form. - Abstract: Graphene platelets were synthesized from graphene oxide by chemical and electrochemical route. Under the chemical method, sodium borohydride and hydrazine chloride were used as reductants to produce graphene. In this paper, a novel and cost effective electrochemical method, which can simplify the process of reduction on a larger scale, is demonstrated. The electrochemical method proposed in this paper produces graphene in powder form with good yield. The atomic force microscopic images confirmed that the graphene samples prepared by all the routes have multilayers of graphene. The electrochemical process provided a new route to make relatively larger area graphene sheets, which will have interest for further patterning applications. Attempt was made to quantify the quantum of reduction using cyclic voltammetry and choronopotentiometry techniques on reduced graphene samples. As a measure in reading the specific capacitance values, a maximum specific capacitance value of 265.3 F/g was obtained in sodium borohydride reduced graphene oxide.

Synthesis of graphene platelets by chemical and electrochemical route

International Nuclear Information System (INIS)

Ramachandran, Rajendran; Felix, Sathiyanathan; Joshi, Girish M.; Raghupathy, Bala P.C.; Jeong, Soon Kwan; Grace, Andrews Nirmala

2013-01-01

Graphical abstract: A schematic showing the overall reduction process of graphite to reduced graphene platelets by chemical and electrochemical route. - Highlights: • Graphene was prepared by diverse routes viz. chemical and electrochemical methods. • NaBH 4 was effective for removing oxygen functional groups from graphene oxide. • Sodium borohydride reduced graphene oxide (SRGO) showed high specific capacitance. • Electrochemical rendered a cheap route for production of graphene in powder form. - Abstract: Graphene platelets were synthesized from graphene oxide by chemical and electrochemical route. Under the chemical method, sodium borohydride and hydrazine chloride were used as reductants to produce graphene. In this paper, a novel and cost effective electrochemical method, which can simplify the process of reduction on a larger scale, is demonstrated. The electrochemical method proposed in this paper produces graphene in powder form with good yield. The atomic force microscopic images confirmed that the graphene samples prepared by all the routes have multilayers of graphene. The electrochemical process provided a new route to make relatively larger area graphene sheets, which will have interest for further patterning applications. Attempt was made to quantify the quantum of reduction using cyclic voltammetry and choronopotentiometry techniques on reduced graphene samples. As a measure in reading the specific capacitance values, a maximum specific capacitance value of 265.3 F/g was obtained in sodium borohydride reduced graphene oxide

Synthesis of Pt nanoparticles on electrochemically reduced graphene oxide by potentiostatic and alternate current methods

Energy Technology Data Exchange (ETDEWEB)

Molina, J.; Fernández, J.; Río, A.I. del; Bonastre, J.; Cases, F., E-mail: fjcases@txp.upv.es

2014-03-01

Reduced graphene oxide (RGO) has been synthesized on Pt wires by means of a potentiodynamic method between + 0.6 V and − 1.4 V for 20 scans. Cyclic voltammetry characterization of the coatings showed the typical capacitative behavior of graphene. Pt nanoparticles were synthesized on Pt–RGO electrodes by means of potentiostatic methods and a comparison between different synthesis potentials (− 0.16, 0, + 0.2 and + 0.4 V) for the same synthesis charge (mC·cm{sup −2}) was established. The electrodes obtained were characterized in 0.5 M H{sub 2}SO{sub 4} solution to observe the characteristic oxidation and reduction processes of the Pt surface. A 0.5 M H{sub 2}SO{sub 4}/0.5 M CH{sub 3}OH solution was used to measure the catalytic properties of the deposits against methanol oxidation. The most appropriate potential to perform the synthesis was 0 V followed by − 0.16 V and + 0.2 V. The morphology of the coatings varied depending on the potential applied as observed by scanning electron microscopy. Alternate current methods were also used to synthesize Pt nanoparticles and compare the results with the traditional potentiostatic method. Different frequencies were used: 0.1, 1, 10, 100, 1000 and 10 000 Hz. Alternate current synthesis is more efficient than traditional potentiostatic methods, obtaining more electroactive coatings with less effective synthesis time. - Highlights: • Reduced graphene oxide has been obtained by electrochemical reduction on Pt wires. • Pt nanoparticles have been obtained potentiostatically at different potentials. • Pt nanoparticles have been obtained by ac methods with different frequencies. • ac synthesis is a better synthesis method than potentiostatic synthesis.

Electrochemical synthesis of polydiphenylamine nanofibrils through AAO template

International Nuclear Information System (INIS)

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

2005-01-01

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

Electrochemical synthesis of polydiphenylamine nanofibrils through AAO template

Energy Technology Data Exchange (ETDEWEB)

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

2005-06-15

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

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

International Nuclear Information System (INIS)

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

2012-01-01

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

Synthesis of TiO2 by electrochemical method from TiCl4 solution as anode material for lithium-ion batteries

International Nuclear Information System (INIS)

Nur, Adrian; Purwanto, Agus; Jumari, Arif; Dyartanti, Endah R.; Sari, Sifa Dian Permata; Hanifah, Ita Nur

2016-01-01

Metal oxide combined with graphite becomes interesting composition. TiO 2 is a good candidate for Li ion battery anode because of cost, availability of sufficient materials, and environmentally friendly. TiO 2 gravimetric capacity varied within a fairly wide range. TiO 2 crystals form highly depends on the synthesis method used. The electrochemical method is beginning to emerge as a valuable option for preparing TiO 2 powders. Using the electrochemical method, the particle can easily be controlled by simply adjusting the imposed current or potential to the system. In this work, the effects of some key parameters of the electrosynthesis on the formation of TiO 2 have been investigated. The combination of graphite and TiO 2 particle has also been studied for lithium-ion batteries. The homogeneous solution for the electrosynthesis of TiO 2 powders was TiCl 4 in ethanol solution. The electrolysis was carried out in an electrochemical cell consisting of two carbon electrodes with dimensions of (5 × 2) cm. The electrodes were set parallel with a distance of 2.6 cm between the electrodes and immersed in the electrolytic solution at a depth of 2 cm. The electrodes were connected to the positive and negative terminals of a DC power supply. The electrosynthesis was performed galvanostatically at 0.5 to 2.5 hours and voltages were varied from 8 to 12 V under constant stirring at room temperature. The resulted suspension was aged at 48 hrs, filtered, dried directly in an oven at 150°C for 2 hrs, washed 2 times, and dried again 60 °C for 6 hrs. The particle product has been used to lithium-ion battery as anode. Synthesis of TiO 2 particle by electrochemical method at 10 V for 1 to 2.5 hrs resulted anatase and rutile phase

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

International Nuclear Information System (INIS)

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

2014-01-01

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

Rapid synthesis of Co, Ni co-doped ZnO nanoparticles: Optical and electrochemical properties

Energy Technology Data Exchange (ETDEWEB)

Romeiro, Fernanda C.; Marinho, Juliane Z.; Lemos, Samantha C.S. [Instituto de Química, Universidade Federal de Uberlândia, 38400-902 Uberlândia, MG (Brazil); Moura, Ana P. de [LIEC, Instituto de Química, Universidade Estadual Paulista, 14800-900 Araraquara, SP (Brazil); Freire, Poliana G. [Instituto de Química, Universidade Federal de Uberlândia, 38400-902 Uberlândia, MG (Brazil); Silva, Luis F. da; Longo, Elson [LIEC, Instituto de Química, Universidade Estadual Paulista, 14800-900 Araraquara, SP (Brazil); Munoz, Rodrigo A.A. [Instituto de Química, Universidade Federal de Uberlândia, 38400-902 Uberlândia, MG (Brazil); Lima, Renata C., E-mail: rclima@iqufu.ufu.br [Instituto de Química, Universidade Federal de Uberlândia, 38400-902 Uberlândia, MG (Brazil)

2015-10-15

We report for the first time a rapid preparation of Zn{sub 1−2x}Co{sub x}Ni{sub x}O nanoparticles via a versatile and environmentally friendly route, microwave-assisted hydrothermal (MAH) method. The Co, Ni co-doped ZnO nanoparticles present an effect on photoluminescence and electrochemical properties, exhibiting excellent electrocatalytic performance compared to undoped ZnO sample. Photoluminescence spectroscopy measurements indicated the reduction of the green–orange–red visible emission region after adding Co and Ni ions, revealing the formation of alternative pathways for the generated recombination. The presence of these metallic ions into ZnO creates different defects, contributing to a local structural disorder, as revealed by Raman spectra. Electrochemical experiments revealed that the electrocatalytic oxidation of dopamine on ZnO attached to multi-walled carbon nanotubes improved significantly in the Co, Ni co-doped ZnO samples when compared to pure ZnO. - Graphical abstract: Rapid synthesis of Co, Ni co-doped ZnO nanoparticles: optical and electrochemical properties. Co, Ni co-doped ZnO hexagonal nanoparticles with optical and electrocatalytic properties were successfully prepared for the first time using a microwave hydrothermal method at mild conditions. - Highlights: • Co{sup 2+} and Ni{sup 2+} into ZnO lattice obtained a mild and environmentally friendly process. • The heating method strongly influences in the growth and shape of the particles. • Short-range defects generated by the ions insertion affects the photoluminescence. • Doped ZnO nanoparticles improve the electrocatalytic properties of pure oxide.

High power Nb-doped LiFePO4 Li-ion battery cathodes; pilot-scale synthesis and electrochemical properties

Science.gov (United States)

Johnson, Ian D.; Blagovidova, Ekaterina; Dingwall, Paul A.; Brett, Dan J. L.; Shearing, Paul R.; Darr, Jawwad A.

2016-09-01

High power, phase-pure Nb-doped LiFePO4 (LFP) nanoparticles are synthesised using a pilot-scale continuous hydrothermal flow synthesis process (production rate of 6 kg per day) in the range 0.01-2.00 at% Nb with respect to total transition metal content. EDS analysis suggests that Nb is homogeneously distributed throughout the structure. The addition of fructose as a reagent in the hydrothermal flow process, followed by a post synthesis heat-treatment, affords a continuous graphitic carbon coating on the particle surfaces. Electrochemical testing reveals that cycling performance improves with increasing dopant concentration, up to a maximum of 1.0 at% Nb, for which point a specific capacity of 110 mAh g-1 is obtained at 10 C (6 min for the charge or discharge). This is an excellent result for a high power cathode LFP based material, particularly when considering the synthesis was performed on a large pilot-scale apparatus.

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

Directory of Open Access Journals (Sweden)

Soon Weng Chong

2016-01-01

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

Low-temperature direct synthesis of mesoporous vanadium nitrides for electrochemical capacitors

Science.gov (United States)

Lee, Hae-Min; Jeong, Gyoung Hwa; Kim, Sang-Wook; Kim, Chang-Koo

2017-04-01

Mesoporous vanadium nitrides are directly synthesized by a one-step chemical precipitation method at a low temperature (70 °C). Structural and morphological analyses reveal that vanadium nitride consist of long and slender nanowhiskers, and mesopores with diameters of 2-5 nm. Compositional analysis confirms the presence of vanadium in the VN structure, along with oxidized vanadium. The cyclic voltammetry and charge-discharge tests indicate that the obtained material stores charges via a combination of electric double-layer capacitance and pseudocapacitance mechanisms. The vanadium nitride electrode exhibits a specific capacitance of 598 F/g at a current density of 4 A/g. After 5000 charge-discharge cycles, the electrode has an equivalent series resistance of 1.42 Ω and retains 83% of its initial specific capacitance. This direct low-temperature synthesis of mesoporous vanadium nitrides is a simple and promising method to achieve high specific capacitance and low equivalent series resistance for electrochemical capacitor applications.

Electrochemical synthesis of highly ordered polypyrrole on copper modified aluminium substrates

International Nuclear Information System (INIS)

Siddaramanna, Ashoka; Saleema, N.; Sarkar, D.K.

2014-01-01

Fabrication of highly ordered conducting polymers on metal surfaces has received a significant interest owing to their potential applications in organic electronic devices. In this context, we have developed a simple method for the synthesis of highly ordered polypyrrole (PPy) on copper modified aluminium surfaces via electrochemical polymerization process. A series of characteristic peaks of PPy evidenced on the infrared spectra of these surfaces confirm the formation of PPy. The X-ray diffraction (XRD) pattern of PPy deposited on copper modified aluminium surfaces also confirmed the deposition of PPy as a sharp and intense peak at 2θ angle of 23° attributable to PPy is observed while this peak is absent on PPy deposited on as-received aluminium surfaces. An atomic model of the interface of PPy/Cu has been presented based on the inter-atomic distance of copper–copper of (1 0 0) plane and the inter-monomer distance of PPy, to describe the ordering of PPy on Cu modified Al surfaces.

Electrochemical synthesis of self-organized TiO2 crystalline nanotubes without annealing

Science.gov (United States)

Giorgi, Leonardo; Dikonimos, Theodoros; Giorgi, Rossella; Buonocore, Francesco; Faggio, Giuliana; Messina, Giacomo; Lisi, Nicola

2018-03-01

This work demonstrates that upon anodic polarization in an aqueous fluoride-containing electrolyte, TiO2 nanotube array films can be formed with a well-defined crystalline phase, rather than an amorphous one. The crystalline phase was obtained avoiding any high temperature annealing. We studied the formation of nanotubes in an HF/H2O medium and the development of crystalline grains on the nanotube wall, and we found a facile way to achieve crystalline TiO2 nanotube arrays through a one-step anodization. The crystallinity of the film was influenced by the synthesis parameters, and the optimization of the electrolyte composition and anodization conditions (applied voltage and time) were carried out. For comparison purposes, crystalline anatase TiO2 nanotubes were also prepared by thermal treatment of amorphous nanotubes grown in an organic bath (ethylene glycol/NH4F/H2O). The morphology and the crystallinity of the nanotubes were studied by field emission gun-scanning electron microscopy (FEG-SEM) and Raman spectroscopy, whereas the electrochemical and semiconducting properties were analyzed by means of linear sweep voltammetry, impedance spectroscopy, and Mott-Schottky plots. X-ray photoelectron spectroscopy (XPS) and ultraviolet photoelectron spectroscopy (UPS) allowed us to determine the surface composition and the electronic structure of the samples and to correlate them with the electrochemical data. The optimal conditions to achieve a crystalline phase with high donor concentration are defined.

Investigation of electrochemical synthesis of ferrate, Part I: Electrochemical behavior of iron and its several alloys in concentrated alkaline solutions

Directory of Open Access Journals (Sweden)

Čekerevac Milan I.

2009-01-01

Full Text Available In recent years, considerable attention has been paid to various applications of Fe(VI due to its unique properties such as oxidizing power, selective reactivity, stability of the salt, and non-toxic decomposition by-products of ferric ion. In environmental remediation processes, Fe(VI has been proposed as green oxidant, coagulant, disinfectant, and antifoulant. Therefore, it is considered as a promising multi-purpose water treatment chemical. Fe(VI has also potential applications in electrochemical energy source, as 'green cathode'. The effectiveness of ferrate as a powerful oxidant in the entire pH range, and its use in environmental applications for the removal of wide range of contaminants has been well documented by several researchers. There is scientific evidence that ferrate can effectively remove arsenic, algae, viruses, pharmaceutical waste, and other toxic heavy metals. Although Fe(VI was first discovered in early eighteen century, detailed studies on physical and chemical properties of Fe(VI had to wait until efficient synthetic and analytical methods of Fe(VI were developed by Schreyer et al. in the 1950s. Actually, there have been developed three ways for the preparation of Fe(VI compounds : the wet oxidation of Fe(II and Fe(III compounds, the dry oxidation of the same, and the electrochemistry method, mainly based on the trans passive oxidation of iron. High purity ferrates Fe(VI can be generated when electrode of the pure iron metal or its alloys are anodized in concentrated alkaline solution. It is known that the efficiency of electrochemical process of Fe(VI production depends on many factors such as current density, composition of anode material, types of electrolyte etc. In this paper, the electrochemical synthesis of ferrate(VI solution by the anodic dissolution of iron and its alloys in concentrated water solution of NaOH and KOH is investigated. The process of transpassive dissolution of iron to ferrate(VI was studied by

Synthesis and electrochemical properties of Na-rich Prussian blue analogues containing Mn, Fe, Co, and Fe for Na-ion batteries

Science.gov (United States)

Bie, Xiaofei; Kubota, Kei; Hosaka, Tomooki; Chihara, Kuniko; Komaba, Shinichi

2018-02-01

Electrochemical performance of Prussian blue analogues (PBAs) as positive electrode materials for non-aqueous Na-ion batteries is known to be highly dependent on their synthesis conditions according to the previous researches. Na-rich PBAs, NaxM[Fe(CN)6]·nH2O where M = Mn, Fe, Co, and Ni, are prepared via precipitation method under the same condition. The structure, chemical composition, morphology, valence of the transition metals, and electrochemical property of these samples are comparatively researched. The PBA with Mn shows large reversible capacity of 126 mAh g-1 in 2.0-4.2 V at a current density of 30 mA g-1 and the highest working voltage owning to high redox potential of Mn2+/3+ in MnN6 and Fe2+/3+ in FeC6. While, the PBA with Ni exhibits the best cyclability and rate performance though only 66 mAh g-1 is delivered. The significant differences in electrochemical behaviors of the PBAs originate from the various properties depending on different transition metals.

The electrochemical synthesis of poly(pyrrole-co-o-anisidine) on 3102 aluminum alloy and its corrosion protection properties

International Nuclear Information System (INIS)

Mert, B. Dogru; Yazici, B.

2011-01-01

Research highlights: → The electrochemical synthesis of strongly adherent, uniform polypyrrole (PPy) and poly(pyrrole-co-o-anisidine) coatings were successfully achieved on 3102 aluminum alloy from 0.1 M monomer (pyrrole and pyrrole:o-anisidine, 8:2) containing oxalic acid by means of the cyclic voltammetry technique. → The results were showed that the water permeation of copolymer coating is lower than PPy. → This study was showed that copolymer is suitable coating for protection of 3102 Al alloy against corrosion. - Abstract: The electrochemical syntheses of polypyrrole (PPy) and poly(pyrrole-co-o-anisidine) were achieved on 3102 aluminum alloy (Al) from 0.1 M monomer (pyrrole:o-anisidine, 8:2) containing 0.4 M oxalic acid solution using the cyclic voltammetry technique. The synthesized films were characterized by FT-IR spectroscopy. The thermal stability of films was determined by thermogravimetric analysis (TGA) technique. Surface morphologies were characterized by scanning electron microscope (SEM) images. The potential of zero charge (pzc) of Al was determined using electrochemical impedance spectroscopy (EIS). The corrosion behavior of samples was investigated with open circuit potential (E ocp )-time, EIS, and anodic polarization techniques. It was found that copolymer coated Al provides better barrier property against of corrosion in 3.5% NaCl solution.

In situ chemical synthesis of ruthenium oxide/reduced graphene oxide nanocomposites for electrochemical capacitor applications.

Science.gov (United States)

Kim, Ji-Young; Kim, Kwang-Heon; Yoon, Seung-Beom; Kim, Hyun-Kyung; Park, Sang-Hoon; Kim, Kwang-Bum

2013-08-07

An in situ chemical synthesis approach has been developed to prepare ruthenium oxide/reduced graphene oxide (RGO) nanocomposites. It is found that as the C/O ratio increases, the number density of RuO2 nanoparticles decreases, because the chemical interaction between the Ru ions and the oxygen-containing functional groups provides anchoring sites where the nucleation of particles takes place. For electrochemical capacitor applications, the microwave-hydrothermal process was carried out to improve the conductivity of RGO in RuO2/RGO nanocomposites. The significant improvement in capacitance and high rate capability might result from the RuO2 nanoparticles used as spacers that make the interior layers of the reduced graphene oxide electrode available for electrolyte access.

Synthesis of naturally-derived macromolecules through simplified electrochemically mediated ATRP

Directory of Open Access Journals (Sweden)

Paweł Chmielarz

2017-11-01

Full Text Available The flavonoid-based macroinitiator was received for the first time by the transesterification reaction of quercetin with 2-bromoisobutyryl bromide. In accordance with the “grafting from” strategy, a naturally-occurring star-like polymer with a polar 3,3',4',5,6-pentahydroxyflavone core and hydrophobic poly(tert-butyl acrylate (PtBA side arms was synthesized via a simplified electrochemically mediated ATRP (seATRP, utilizing only 78 ppm by weight (wt of a catalytic CuII complex. To demonstrate the possibility of temporal control, seATRP was carried out utilizing a multiple-step potential electrolysis. The rate of the polymerizations was well-controlled by applying optimal potential values during preparative electrolysis to prevent the possibility of intermolecular coupling of the growing polymer arms. This appears to be the first report using on-demand seATRP for the synthesis of QC-(PtBA-Br5 pseudo-star polymers. The naturally-derived macromolecules showed narrow MWDs (Đ = 1.08–1.11. 1H NMR spectral results confirm the formation of quercetin-based polymers. These new flavonoid-based polymer materials may find applications as antifouling coatings and drug delivery systems.

Process Design for Size-Controlled Flame Spray Synthesis of Li4Ti5O12 and Electrochemical Performance

Directory of Open Access Journals (Sweden)

Waser Oliver

2017-03-01

Full Text Available Inexpensive synthesis of electroceramic materials is required for efficient energy storage. Here the design of a scalable process, flame spray pyrolysis (FSP, for synthesis of size-controlled nanomaterials is investigated focusing on understanding the role of air entrainment (AE during their aerosol synthesis with emphasis on battery materials. The AE into the enclosed FSP reactor is analysed quantitatively by computational fluid dynamics (CFD and calculated temperatures are verified by Fourier transform infrared spectroscopy (FTIR. Various Li4Ti5O12 (LTO particle compositions are made and characterized by N2 adsorption, electron microscopy and X-ray diffraction while the electrochemical performance of LTO is tested at various charging rates. Increasing AE decreases recirculation in the enclosing tube leading to lower reactor temperatures and particle concentrations by air dilution as well as shorter and narrower residence time distributions. As a result, particle growth by coagulation - coalescence decreases leading to smaller primary particles that are mostly pure LTO exhibiting high C-rate performance with more than 120 mAh/g galvanostatic specific charge at 40C, outperforming commercial LTO. The effect of AE on FSP-made particle characteristics is demonstrated also in combustion synthesis of LiFePO4 and ZrO2.

Electrochemical synthesis of CORE-shell magnetic nanowires

KAUST Repository

Ovejero, Jesú s G.; Bran, Cristina; Vidal, Enrique Vilanova; Kosel, Jü rgen; Morales, Marí a P.; Vazquez, Manuel

2015-01-01

(Fe, Ni, CoFe) @ Au core-shell magnetic nanowires have been synthesized by optimized two-step potentiostatic electrodeposition inside self-assembled nanopores of anodic aluminium templates. The optimal electrochemical parameters (e.g., potential

Synthesis and Electrochemical Performance of SiOC-Carbon Nanotube Composite Coatings

Science.gov (United States)

Bhandavat, Romil; Cologna, Marco; Raj, Rishi; Singh, Gurpreet

2012-02-01

Rechargeable battery anodes made from crystalline Si-based nanostructures have been shown to possess high experimental first cycle capacities (3000 mAh/g), but face challenges in sustaining these capacities beyond initial cycles mainly due to large volume expansion (400 percent) and chemical degradation (pulverization). Polymer-derived ceramic SiOC due to its high thermodynamic stability and nano domain structure could present a viable alternative. Additionally, functionalization of SiOC with carbon nanotubes could result in increased electronic and ionic conductivities in the ceramic. Here, we demonstrate synthesis and electrochemical characterization of SiOC-CNT composite coatings for use in Li-ion battery anode. Materials characterization performed using electron microscopy, Infrared (FT-IR), and X-ray photoelectron spectroscopy suggests non-covalent functionalization of CNT with oxygen moieties in SiOC. Sustained battery capacities of over 700 mAh/g and first cycle columbic efficiencies of about 75 percent were achieved. Future work will involve determination of lithium ion intercalation sites characterized by electron microscopy whereas cyclic voltammetry analysis will access the sequential change in anode chemistry.

Fused 1,2,3-Dithiazoles: Convenient Synthesis, Structural Characterization, and Electrochemical Properties

Directory of Open Access Journals (Sweden)

Lidia S. Konstantinova

2016-05-01

Full Text Available A new general protocol for synthesis of fused 1,2,3-dithiazoles by the reaction of cyclic oximes with S2Cl2 and pyridine in acetonitrile has been developed. The target 1,2,3-dithiazoles fused with various carbocycles, such as indene, naphthalenone, cyclohexadienone, cyclopentadiene, and benzoannulene, were selectively obtained in low to high yields. In most cases, the hetero ring-closure was accompanied by chlorination of the carbocyclic moieties. With naphthalenone derivatives, a novel dithiazole rearrangement (15→13 featuring unexpected movement of the dithiazole ring from α- to β-position, with respect to keto group, was discovered. Molecular structure of 4-chloro-5H-naphtho[1,2-d][1,2,3]dithiazol-5-one 13 was confirmed by single-crystal X-ray diffraction. Electrochemical properties of 13 were studied by cyclic voltammetry and a complex behavior was observed, most likely including hydrodechlorination at a low potential.

Electrochemical synthesis of gold nanorods in track-etched polycarbonate membrane using removable mercury cathode

International Nuclear Information System (INIS)

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

2012-01-01

The electrochemical template synthesis of gold nanorods within the cylindrical pores of track-etched polycarbonate (PC) membrane using a removable mercury cathode is reported. The novelty of this new approach is that it eliminates the requirement of coating an approximately 500 nm–1 μm-thick metallic layer, as conducting substrate, onto one surface of the insulating template membrane by the sputter deposition technique. A two-compartment electrochemical cell was designed and used for this work. The PC membrane was placed between the two compartments separating the aqueous solution of HAuCl 4 from mercury. Mercury, filled in one of the compartments, is in contact with one surface of the membrane (similar to sputter-deposited metallic layer) and serves as the conducting substrate/cathode for the electrochemical deposition of gold in the nanopores of track-etched PC membrane. Once the electrodeposition is completed, the mercury and the HAuCl 4 solution are removed from the compartments, and a malleable track-etched PC membrane embedded with free-standing gold nanorods is obtained. The ensemble of the metal nanorods grown in the template membrane is not attached to any conducting substrate, and gold nanorods can be freed from the template membrane after the dissolution. The Au-deposited PC membrane and free-standing Au nanorods were characterized by EDXRF, XRD, UV–Visible spectroscopy, AFM, and FEG-TEM. The EDXRF and XRD studies confirmed the deposition of the face-centered cubic phase of Au in the pores of the PC membrane. The TEM studies showed the formation of a cigar-shaped gold nanorod in the cylindrical pores of the PC membrane. The diameter of gold nanorods ranges from 100 to 200 nm. The new approach is simple, cost-effective, and saves time.

Electrochemical synthesis of CORE-shell magnetic nanowires

KAUST Repository

Ovejero, Jesús G.

2015-04-16

(Fe, Ni, CoFe) @ Au core-shell magnetic nanowires have been synthesized by optimized two-step potentiostatic electrodeposition inside self-assembled nanopores of anodic aluminium templates. The optimal electrochemical parameters (e.g., potential) have been firstly determined for the growth of continuous Au nanotubes at the inner wall of pores. Then, a magnetic core was synthesized inside the Au shells under suitable electrochemical conditions for a wide spectrum of single elements and alloy compositions (e.g., Fe, Ni and CoFe alloys). Novel opportunities offered by such nanowires are discussed particularly the magnetic behavior of (Fe, Ni, CoFe) @ Au core-shell nanowires was tested and compared with that of bare TM nanowires. These core-shell nanowires can be released from the template so, opening novel opportunities for biofunctionalization of individual nanowires.

Synthesis of palladium@gold nanoalloys/nitrogen and sulphur-functionalized multiple graphene aerogel for electrochemical detection of dopamine

Energy Technology Data Exchange (ETDEWEB)

Li, Ruiyi; Yang, Tingting [School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122 (China); Li, Zaijun, E-mail: zaijunli@jiangnan.edu.cn [School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122 (China); Key Laboratory of Food Colloids and Biotechnology, Ministry of Education, Wuxi 214122 (China); Gu, Zhiguo; Wang, Guangli; Liu, Junkang [School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122 (China)

2017-02-15

Integration of noble metal nanomaterials on graphene nanosheets potentially paves one way to improve their electronic, chemical and electrochemical properties. The study reported synthesis of palladium@gold nanoalloys/nitrogen and sulphur-functionalized multiple graphene aerogel composite (Pd@Au/N,S-MGA). The as-prepared composite offers a well-defined three-dimensional architecture with rich of mesopores. The Pd@Au nanoalloys were dispersed on the graphene framework networks and their active sites were fully exposed. The unique structure achieves to ultra high electron/ion conductivity, electrocatalytic activity and structural stability. The sensor based on the Pd@Au/N,S-MGA creates ultrasensitive electrochemical response towards dopamine due to significantly electrochemical synergy between Pd, Au and N,S-MGA. Its differential pulse voltammetric signal linearly increases with the increase of dopamine concentration in the range from 1.0 × 10{sup −9} M to 4.0 × 10{sup −5} M with the detection limit of 3.6 × 10{sup −10} M (S/N = 3). The analytical method provides the advantage of sensitivity, reproducibility, rapidity and long-term stability. It has been successfully applied in the detection of trace dopamine in biological samples. The study also opens a window on the electronic properties of graphene aerogel and metal nanomaterials as well their nanohybrids to meet needs of further applications as nanoelectronics in diagnosis, bioanalysis and catalysis. - Graphical abstract: We reported a new palladium@gold nanoalloys/nitrogen and sulphur-functionalized multiple graphene aerogel. The sensor based on the nanohybrid exhibits ultrahigh sensitivity, reproducibility and stability to electrochemical detection of dopamine. - Highlights: • We reported Pd@A/nitrogen and sulphur-functionalized multiple graphene aerogel. • The nanohybrid offers unique three-dimensional architecture with rich of mesopores. • The architecture achieve to ultrahigh

Synthesis of palladium@gold nanoalloys/nitrogen and sulphur-functionalized multiple graphene aerogel for electrochemical detection of dopamine

International Nuclear Information System (INIS)

Li, Ruiyi; Yang, Tingting; Li, Zaijun; Gu, Zhiguo; Wang, Guangli; Liu, Junkang

2017-01-01

Integration of noble metal nanomaterials on graphene nanosheets potentially paves one way to improve their electronic, chemical and electrochemical properties. The study reported synthesis of palladium@gold nanoalloys/nitrogen and sulphur-functionalized multiple graphene aerogel composite (Pd@Au/N,S-MGA). The as-prepared composite offers a well-defined three-dimensional architecture with rich of mesopores. The Pd@Au nanoalloys were dispersed on the graphene framework networks and their active sites were fully exposed. The unique structure achieves to ultra high electron/ion conductivity, electrocatalytic activity and structural stability. The sensor based on the Pd@Au/N,S-MGA creates ultrasensitive electrochemical response towards dopamine due to significantly electrochemical synergy between Pd, Au and N,S-MGA. Its differential pulse voltammetric signal linearly increases with the increase of dopamine concentration in the range from 1.0 × 10"−"9 M to 4.0 × 10"−"5 M with the detection limit of 3.6 × 10"−"1"0 M (S/N = 3). The analytical method provides the advantage of sensitivity, reproducibility, rapidity and long-term stability. It has been successfully applied in the detection of trace dopamine in biological samples. The study also opens a window on the electronic properties of graphene aerogel and metal nanomaterials as well their nanohybrids to meet needs of further applications as nanoelectronics in diagnosis, bioanalysis and catalysis. - Graphical abstract: We reported a new palladium@gold nanoalloys/nitrogen and sulphur-functionalized multiple graphene aerogel. The sensor based on the nanohybrid exhibits ultrahigh sensitivity, reproducibility and stability to electrochemical detection of dopamine. - Highlights: • We reported Pd@A/nitrogen and sulphur-functionalized multiple graphene aerogel. • The nanohybrid offers unique three-dimensional architecture with rich of mesopores. • The architecture achieve to ultrahigh electron

Hydrothermal synthesis of mesoporous metal oxide arrays with enhanced properties for electrochemical energy storage

International Nuclear Information System (INIS)

Xiao, Anguo; Zhou, Shibiao; Zuo, Chenggang; Zhuan, Yongbing; Ding, Xiang

2015-01-01

Highlights: • NiO mesoporous nanowall arrays are prepared via hydrothermal method. • Mesoporous nanowall arrays are favorable for fast ion/electron transfer. • NiO mesoporous nanowall arrays show good supercapacitor performance. - Abstract: Mesoporous nanowall NiO arrays are prepared by a facile hydrothermal synthesis method with a following annealing process. The NiO nanowall shows continuous mesopores ranging from 5 to 10 nm and grows vertically on the substrate forming a porous net-like structure with macropores of 20–300 nm. A plausible mechanism is proposed for the growth of mesoporous nanowall NiO arrays. As cathode material of pseudocapacitors, the as-prepared mesoporous nanowall NiO arrays show good pseudocapacitive performances with a high capacitance of 600 F g −1 at 2 A g −1 and impressive high-rate capability with a specific capacitance of 338 F g −1 at 40 A g −1 . In addition, the mesoporous nanowall NiO arrays possess good cycling stability. After 6000 cycles at 2 A g −1 , a high capacitance of 660 F g −1 is attained, and no obvious degradation is observed. The good electrochemical performance is attributed to its highly porous morphology, which provides large reaction surface and short ion diffusion paths, leading to enhanced electrochemical properties

Characterization and optimization of cathodic conditions for H2O2 synthesis in microbial electrochemical cells.

Science.gov (United States)

Sim, Junyoung; An, Junyeong; Elbeshbishy, Elsayed; Ryu, Hodon; Lee, Hyung-Sool

2015-11-01

Cathode potential and O2 supply methods were investigated to improve H2O2 synthesis in an electrochemical cell, and optimal cathode conditions were applied for microbial electrochemical cells (MECs). Using aqueous O2 for the cathode significantly improved current density, but H2O2 conversion efficiency was negligible at 0.3-12%. Current density decreased for passive O2 diffusion to the cathode, but H2O2 conversion efficiency increased by 65%. An MEC equipped with a gas diffusion cathode was operated with acetate medium and domestic wastewater, which presented relatively high H2O2 conversion efficiency from 36% to 47%, although cathode overpotential was fluctuated. Due to different current densities, the maximum H2O2 production rate was 141 mg H2O2/L-h in the MEC fed with acetate medium, but it became low at 6 mg H2O2/L-h in the MEC fed with the wastewater. Our study clearly indicates that improving anodic current density and mitigating membrane fouling would be key parameters for large-scale H2O2-MECs. Copyright © 2015 Elsevier Ltd. All rights reserved.

Bio-electrochemical synthesis of commodity chemicals by ...

Indian Academy of Sciences (India)

2016-08-02

Aug 2, 2016 ... be exploited in a bio-electrochemical system for current generation or to provide ..... fiber was desorbed directly to GC injector for 3 min. This ..... The authors are grateful to COMSATS Institute of Information. Technology ...

Synthesis and characterization of electrochemically-reduced graphene

Indian Academy of Sciences (India)

Keywords. Graphene; electrochemical deposition; heat treatment; conductivity. 1. Introduction ... solar cells (Wu et al 2008; Sima et al 2011), molecular gas sensors ... solved in deionized (DI) water to obtain 0·01 M of electrolyte solution (Su et ...

Synthesis and electrochemical properties of porous double-shelled Mn2O3 hollow microspheres as a superior anode material for lithium ion batteries

International Nuclear Information System (INIS)

Qiao, Yu; Yu, Yan; Jin, Yi; Guan, Yi-Biao; Chen, Chun-Hua

2014-01-01

Highlights: • Double-shelled Mn 2 O 3 hollow microspheres are prepared by a multi-step. • synthesis procedure. • Solid, hollow and yolk-structured Mn 2 O 3 spheres are prepared for comparison. • The double-shelled hollow Mn 2 O 3 is superior in electrochemical properties. - Abstract: By means of a specially designed multi-step synthesis procedure involving steps of precipitation, controlled oxidation, selective etching and calcination, porous double-shelled Mn 2 O 3 hollow microspheres are synthesized. Solid, hollow and yolk-structured Mn 2 O 3 are also similarly synthesized for comparison. X-ray diffraction, scanning and transmission electron microscopies, IR spectroscopy, thermogravimetry, and Brunauer-Emmett-Teller measurements are employed to investigate their structures and compositions. Galvanostatic cell cycling and impedance spectroscopy are used to characterize the electrochemical properties of Mn 2 O 3 /Li cells. The results show that the hierarchical hollow structured (double-shelled, hollow and yolk-structured) Mn 2 O 3 anode materials deliver higher reversible capacities and excellent cycling stabilities than the solid Mn 2 O 3 . Moreover, among the three hierarchical hollow structured samples, the double shelled sample possesses the best cycling performance, especially at a high current density

Synthesis and characterization of electrochemically-reduced graphene

Indian Academy of Sciences (India)

Graphene has superior electrical conductivity than graphite and other allotropes of carbon because of its high surface area and chemical tolerance. Electrochemically processed graphene sheets were obtained through the reduction of graphene oxide from hydrazine hydrate. The prepared samples were heated to different ...

Synthesis and characterization of dioxouranium (VI) complexes of Schiff bases derived from isatin, isovanillin and o-vanillin

International Nuclear Information System (INIS)

Singh, Kavita; Agarwala, B.V.; Naganagowda, G.A.

1996-01-01

Three Schiff bases viz. isatin semicarbazone, isovanillin thiosemicarbazone, o-vanillin para-anisidine and their dioxouranium (VI) complexes have been synthesised and characterized by elemental analysis, IR and NMR spectral studies. (author). 19 refs., 1 tab

Synthesis of TiO{sub 2} by electrochemical method from TiCl{sub 4} solution as anode material for lithium-ion batteries

Energy Technology Data Exchange (ETDEWEB)

Nur, Adrian, E-mail: adriannur@staff.uns.ac.id; Purwanto, Agus; Jumari, Arif; Dyartanti, Endah R.; Sari, Sifa Dian Permata; Hanifah, Ita Nur [Research Group of Advanced Material, Department of Chemical Engineering, Sebelas Maret University, Jl. Ir. Sutami 36 A Kentingan, Surakarta Indonesia 57126 (Indonesia)

2016-02-08

Metal oxide combined with graphite becomes interesting composition. TiO{sub 2} is a good candidate for Li ion battery anode because of cost, availability of sufficient materials, and environmentally friendly. TiO{sub 2} gravimetric capacity varied within a fairly wide range. TiO{sub 2} crystals form highly depends on the synthesis method used. The electrochemical method is beginning to emerge as a valuable option for preparing TiO{sub 2} powders. Using the electrochemical method, the particle can easily be controlled by simply adjusting the imposed current or potential to the system. In this work, the effects of some key parameters of the electrosynthesis on the formation of TiO{sub 2} have been investigated. The combination of graphite and TiO{sub 2} particle has also been studied for lithium-ion batteries. The homogeneous solution for the electrosynthesis of TiO{sub 2} powders was TiCl{sub 4} in ethanol solution. The electrolysis was carried out in an electrochemical cell consisting of two carbon electrodes with dimensions of (5 × 2) cm. The electrodes were set parallel with a distance of 2.6 cm between the electrodes and immersed in the electrolytic solution at a depth of 2 cm. The electrodes were connected to the positive and negative terminals of a DC power supply. The electrosynthesis was performed galvanostatically at 0.5 to 2.5 hours and voltages were varied from 8 to 12 V under constant stirring at room temperature. The resulted suspension was aged at 48 hrs, filtered, dried directly in an oven at 150°C for 2 hrs, washed 2 times, and dried again 60 °C for 6 hrs. The particle product has been used to lithium-ion battery as anode. Synthesis of TiO{sub 2} particle by electrochemical method at 10 V for 1 to 2.5 hrs resulted anatase and rutile phase.

ELECTROCHEMICAL PROMOTED CATALYSIS: TOWARDS PRACTICAL UTILIZATION

Directory of Open Access Journals (Sweden)

DIMITRIOS TSIPLAKIDES

2008-07-01

Full Text Available Electrochemical promotion (EP of catalysis has already been recognized as “a valuable development in catalytic research” (J. Pritchard, 1990 and as “one of the most remarkable advances in electrochemistry since 1950” (J. O’M. Bockris, 1996. Laboratory studies have clearly elucidated the phenomenology of electrochemical promotion and have proven that EP is a general phenomenon at the interface of catalysis and electrochemistry. The major progress toward practical utilization of EP is surveyed in this paper. The focus is given on the electropromotion of industrial ammonia synthesis catalyst, the bipolar EP and the development of a novel monolithic electropromoted reactor (MEPR in conjunction with the electropromotion of thin sputtered metal films. Future perspectives of electrochemical promotion applications in the field of hydrogen technologies are discussed.

Enhancing graphene/CNT based electrochemical detection using magneto-nanobioprobes

OpenAIRE

sprotocols

2015-01-01

Authors: Priyanka Sharma, V Bhalla, E Senthil Prasad, V Dravid, G Shekhawat & C. Raman Suri ### Abstract This protocol describes an optimized signal amplification strategy to develop an ultra-sensitive magneto-electrochemical biosensing platform. The new protocol combines the advantages of carbon nanotube (CNT) and reduced graphene oxide (rGO) together with electrochemical bursting of magnetic nanoparticles. The method involves synthesis of gold-iron (Au/Fe) nano-structures function...

Controllable synthesis of porous LiFePO4 for tunable electrochemical Li-insertion performance

International Nuclear Information System (INIS)

Tian, Xiaohui; Zhou, Yingke; Wu, Guan; Wang, Pengcheng; Chen, Jian

2017-01-01

Highlights: • A templated freeze-drying method is developed to prepare the porous LiFePO 4 . • The pore size and porosity can be controlled by adjusting the conditions. • The effects of the porous properties on the Li-insertion performances are studied. • The optimized composite presents excellent specific capacity and rate capability. - Abstract: A templated freeze-drying method is developed to prepare the porous LiFePO 4 materials with the controlled pore size and porosity, by conveniently adjusting the size and content of the template in the precursor solution. The morphology and structure of the porous LiFePO 4 materials are characterized and the relavant electrochemical lithium-insertion performances are systematically studied. It’s found that the porous characteristics play a critical role in the lithium-ion intercalation processes and significantly affect the power capability of LiFePO 4 . The optimized porous LiFePO 4 material presents remarkable specific capacity (167 mAh g −1 at 0.1 C), rate capability (151 mAh g −1 at 1 C and 110 mAh g −1 at 10 C) and cycling stability (99.3% retention after 300 cycles at 1 C). These findings demonstrate that the electrochemical performance of the electrode material can be purposely tuned and remarkably improved by the rational design and introduction of the suitable pores, which open up new strategies for the synthesis of advanced porous materials for the lithium-ion power battery applications.

Synthesis and Electrochemical Study of a TCAA Derivative – A potential bipolar redox-active material

International Nuclear Information System (INIS)

Hagemann, Tino; Winsberg, Jan; Wild, Andreas; Schubert, Ulrich S.

2017-01-01

The 2,3,7,8-tetracyano-1,4,5,6,9,10-hexazaanthracene (TCAA) derivatives represent an interesting substance class for future research on organic electronic devices, such as solar cells, organic batteries or redox-flow batteries (RFBs). Because of their multivalent redox behavior they are potentially “bipolar”, usable both as cathode and anode activ charge-storage materials. Furthermore, they show a strong absorption and fluorescence behavior both in solution and solid state, rendering them a promising emitter for electroluminescence devices, like lamps or displays. In order to evaluate a TCAA for electrochemical applications the derivative 2,3,7,8-tetracyano-5,10-diphenyl-5,10-dihydrodipyrazino[2,3-b:2′,3′-e] pyrazine (2) was synthesized in two straightforward synthesis steps. The electrochemical behavior of 2 was initially determined by density functional theory (DFT) calculation and afterwards investigated via rotating disc electrode (RDE), UV–vis–NIR spectroelectrochemical as well as cyclic voltammetry (CV) measurements. It features a quasi-reversible oxidation and re-reduction at E ½ = 1.42 V vs. Fc + /Fc with a peak split of 96 mV and a quasi-reversible reduction and re-oxidation at E ½ = −1.49 V vs. Fc + /Fc with a peak split of 174 mV, which lead to a theoretical potential difference of 2.91 V.

Synthesis of microsphere silicon carbide/nanoneedle manganese oxide composites and their electrochemical properties as supercapacitors

Science.gov (United States)

Kim, Myeongjin; Yoo, Youngjae; Kim, Jooheon

2014-11-01

Synthesis of microsphere silicon carbide/nanoneedle MnO2 (SiC/N-MnO2) composites for use as high-performance materials in supercapacitors is reported herein. The synthesis procedure involves the initial treatment of silicon carbide (SiC) with hydrogen peroxide to obtain oxygen-containing functional groups to provide anchoring sites for connection of SiC and the MnO2 nanoneedles (N-MnO2). MnO2 nanoneedles are subsequently formed on the SiC surface. The morphology and microstructure of the as-prepared composites are characterized via X-ray diffractometry, field-emission scanning electron microscopy, thermogravimetric analysis, and X-ray photoelectron spectroscopy. The characterizations indicate that MnO2 nanoneedles are homogeneously formed on the SiC surface in the composite. The capacitive properties of the as-prepared SiC/N-MnO2 electrodes are evaluated using cyclic voltammetry, galvanostatic charge/discharge testing, and electrochemical impedance spectroscopy in a three-electrode experimental setup using a 1-M Na2SO4 aqueous solution as the electrolyte. The SiC/N-MnO2(5) electrode, for which the MnO2/SiC feed ratio is 5:1, displays a specific capacitance as high as 273.2 F g-1 at 10 mV s-1.

Electrochemical redox processes involving soluble cerium species

International Nuclear Information System (INIS)

Arenas, L.F.; Ponce de León, C.; Walsh, F.C.

2016-01-01

Highlights: • The relevance of cerium in laboratory and industrial electrochemistry is considered. • The history of fundamental electrochemical studies and applications is considered. • The chemistry, redox thermodynamics and electrode kinetics of cerium are summarised. • The uses of cerium ions in synthesis, energy storage, analysis and environmental treatment are illustrated. • Research needs and development perspectives are discussed. - Abstract: Anodic oxidation of cerous ions and cathodic reduction of ceric ions, in aqueous acidic solutions, play an important role in electrochemical processes at laboratory and industrial scale. Ceric ions, which have been used for oxidation of organic wastes and off-gases in environmental treatment, are a well-established oxidant for indirect organic synthesis and specialised cleaning processes, including oxide film removal from tanks and process pipework in nuclear decontamination. They also provide a classical reagent for chemical analysis in the laboratory. The reversible oxidation of cerous ions is an important reaction in the positive compartment of various redox flow batteries during charge and discharge cycling. A knowledge of the thermodynamics and kinetics of the redox reaction is critical to an understanding of the role of cerium redox species in these applications. Suitable choices of electrode material (metal or ceramic; coated or uncoated), geometry/structure (2-or 3-dimensional) and electrolyte flow conditions (hence an acceptable mass transport rate) are critical to achieving effective electrocatalysis, a high performance and a long lifetime. This review considers the electrochemistry of soluble cerium species and their diverse uses in electrochemical technology, especially for redox flow batteries and mediated electrochemical oxidation.

Graphene directed architecture of fine engineered nanostructures with electrochemical applications

DEFF Research Database (Denmark)

Hou, Chengyi; Zhang, Minwei; Halder, Arnab

2017-01-01

, and polymers has led to the possibility to create new electroactive and multifunctional nanostructures, which can serve as promising material platforms for electrochemical purposes. However, the precise control and fine-tuning of material structures and properties are still challenging and in demand...... classified nanostructures, including metallic nanostructures, self-assembled organic and supramolecular structures, and fine engineered metal oxides. In these cases, graphene templates either sacrificed during templating synthesis or retained as support for final products. We also discuss remained challenges....... In this review, we aim to highlight some recent efforts devoted to rational design, assembly and fine engineering of electrochemically active nanostructures using graphene or/and its derivatives as soft templates for controlled synthesis and directed growth. We organize the contents according to the chemically...

Facile synthesis of reduced graphene oxide nanosheets by a sodium diphenylamine sulfonate reduction process and its electrochemical property

International Nuclear Information System (INIS)

Ji, Yunzhou; Liu, Qi; Cheng, Meiling; Lai, Lifang; Li, Zhanfeng; Peng, Yuxin; Yang, Yong

2013-01-01

We report a new method to convert graphene oxide (GO) to stable colloidal dispersion of reduced graphene oxide nanosheets (RGONS) using sodium diphenylamine sulfonate (SDAS) as a reductant, as well as itself and its redox product as the stabilizer. The as-prepared RGONS have been characterized by X-ray diffraction, Fourier transform infrared spectroscopy, UV–visible spectroscopy, thermo-gravimetric analysis, scanning and transmission electron microscopy, X-ray photoelectron spectroscopy, atomic force microscopy and Raman spectroscopy. The results indicate that the bulk of oxygen-containing functional groups from GO have been removed. Based on the cyclic voltammogram (CV) analyses, it is found that the RGONS-based material exhibits better electrochemical activity in sensing ascorbic acid than GO. The simple method provides a new efficient route for the synthesis of water-soluble RGONS on a large scale and novel composites. - Highlights: • We report a new environment-friendly reductant for the reduction of graphene oxide. • The reduction process needn't use other stabilizer except for using reductant. • The reduced graphene oxide nanosheet (RGONS) aqueous dispersion is stable. • The RGONS shows a high electrochemical activity in sensing ascorbic acid

Low-temperature direct synthesis of mesoporous vanadium nitrides for electrochemical capacitors

Energy Technology Data Exchange (ETDEWEB)

Lee, Hae-Min [Institute of NT-IT Fusion Technology, Ajou University, 206 Worldcup-ro, Yeongtong-gu, Suwon 16499 (Korea, Republic of); Jeong, Gyoung Hwa [Department of Chemistry, Ulsan National Institute of Science and Technology (UNIST), Banyeon 100, Ulsan 44919 (Korea, Republic of); Kim, Sang-Wook [Department of Molecular Science and Technology, Ajou University, 206 Worldcup-ro, Yeongtong-gu, Suwon 16499 (Korea, Republic of); Kim, Chang-Koo, E-mail: changkoo@ajou.ac.kr [Department of Chemical Engineering and Department of Energy Systems Research, Ajou University, 206 Worldcup-ro, Yeongtong-gu, Suwon 16499 (Korea, Republic of)

2017-04-01

Highlights: • Vanadium nitrides were directly synthesized by a one-step chemical precipitation method. • This method was carried out at a low temperature of 70 °C. • Vanadium nitrides had a specific capacitance of 598 F/g. • The equivalent series resistance of the vanadium nitride electrode was 1.42 Ω after 5000 cycles. - Abstract: Mesoporous vanadium nitrides are directly synthesized by a one-step chemical precipitation method at a low temperature (70 °C). Structural and morphological analyses reveal that vanadium nitride consist of long and slender nanowhiskers, and mesopores with diameters of 2–5 nm. Compositional analysis confirms the presence of vanadium in the VN structure, along with oxidized vanadium. The cyclic voltammetry and charge-discharge tests indicate that the obtained material stores charges via a combination of electric double-layer capacitance and pseudocapacitance mechanisms. The vanadium nitride electrode exhibits a specific capacitance of 598 F/g at a current density of 4 A/g. After 5000 charge-discharge cycles, the electrode has an equivalent series resistance of 1.42 Ω and retains 83% of its initial specific capacitance. This direct low-temperature synthesis of mesoporous vanadium nitrides is a simple and promising method to achieve high specific capacitance and low equivalent series resistance for electrochemical capacitor applications.

One-step and low-temperature synthesis of iodine-doped graphene and its multifunctional applications for hydrogen evolution reaction and electrochemical sensing

International Nuclear Information System (INIS)

Chu, Ke; Wang, Fan; Zhao, Xiao-lin; Wei, Xiao-ping; Wang, Xin-wei; Tian, Ye

2017-01-01

Iodine (I) has emerged as a powerful heteroatom dopant for efficiently tailoring the electrocatalytic properties of graphene. However, the preparation methods of I-doped graphene (I-G) and its electrocatalysis applications remain largely unexplored. Herein, a one-step and low-temperature hydrothermal approach was developed for the successful synthesis of I-G with a high I-doping level (0.52 at.%). The resulting I-G was then applied as a metal-free catalyst for hydrogen evolution reaction (HER) and electrochemical sensing. It was shown that the I-G exhibited a dramatically enhanced HER activity compared to undoped graphene, attributed to the critical role of I-doping in offering large exposed active sites and high electron transfer capability. Furthermore, I-G also displayed attractive sensing performances for highly sensitive and selective detection of dopamine. These findings demonstrate that the hydrothermally synthesized I-G can be a promising electrocatalyst for multifunctional applications in water-splitting and electrochemical sensing.

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

International Nuclear Information System (INIS)

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

2006-01-01

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

Magnetic-field-assisted synthesis of Co{sub 3}O{sub 4} nanoneedles with superior electrochemical capacitance

Energy Technology Data Exchange (ETDEWEB)

Zhu, Tao; Xie, Yan; Zhang, Guoxiong; He, Zhenni; Lu, Yisheng; Guo, Haibo [Shanghai University, Department of Electronic Information Materials, School of Materials Science and Engineering (China); Lin, Chuan [GE Global Research, China Technology Center (China); Chen, Yigang, E-mail: yigangchen@shu.edu.cn [Shanghai University, Department of Electronic Information Materials, School of Materials Science and Engineering (China)

2015-12-15

Nanostructured Co{sub 3}O{sub 4} films have been deposited on nickel foam in a magnetic-field-assisted hydrothermal process followed by annealing in air. The magnetic field strength is varied to study its relationship with nanostructures, morphology, and electrochemical properties of the Co{sub 3}O{sub 4} electrodes. The Co{sub 3}O{sub 4} films synthesized in the weak magnetic fields consist of dispersed nanoneedles, which are different from clustered nanoneedles when the magnetic field is absent. Moreover, the magnetic fields (of several millitesla) induced substantial changes in the nanostructures and electrochemical properties of the Co{sub 3}O{sub 4} films. A possible formation mechanism of Co{sub 3}O{sub 4} nanoneedles is proposed by comparing the morphologies and nanostructures of the films synthesized with and without the magnetic fields. Among these electrodes, the optimal one has a high specific capacitance (970.8 F g{sup −1} at 0.5 A g{sup −1}), good power capability (847.5 F g{sup −1} at 6.0 A g{sup −1}), and an excellent retention ratio (93.7 % over 1000 cycles). All these impressive results demonstrate that magnetic fields may be an economic and effective tool in hydrothermal synthesis of Co{sub 3}O{sub 4} electrodes for high-performance supercapacitors.

MnWO{sub 4} nanocapsules: Synthesis, characterization and its electrochemical sensing property

Energy Technology Data Exchange (ETDEWEB)

Muthamizh, Selvamani; Suresh, Ranganathan; Giribabu, Krishnamoorthy; Manigandan, Ramadoss; Praveen Kumar, Sivakumar; Munusamy, Settu; Narayanan, Vengidusamy, E-mail: vnnara@yahoo.co.in

2015-01-15

Highlights: • Synthesis of MnWO{sub 4} nanocapsules without use of any other external reagent. • High crystalline MnWO{sub 4} was obtained with phase purity. • Electrochemical sensing platform based on MnWO{sub 4} for sensing quercetin. • Micromolar detection ability of MnWO{sub 4} modified GCE. - Abstract: Manganese tungstate (MnWO{sub 4}) was synthesized by surfactant free precipitation method. MnWO{sub 4} was characterized by using various spectroscopic techniques. The phase, crystalline nature and the morphological analysis were carried out using XRD, scanning electron microscopy (SEM), and high resolution transmission electron microscopy (HR-TEM). Further, FT-IR, Raman, and DRS-UV–Vis spectral analysis were carried out in order to ascertain the optical property and the presence of functional groups. From the analysis, the morphology of the MnWO{sub 4} was observed to be in capsules with breadth and thickness were in nm range. The oxidation state of tungsten (W), and manganese (Mn) were investigated using X-ray photo electron spectroscopy (XPS) and electron paramagnetic resonance spectroscopy (EPR). The synthesized MnWO{sub 4} nanocapsules were used to modify glassy carbon electrode (GCE) to detect quercetin.

Synthesis, characterization and electrochemical properties of the V2O5.nH2O/AlO(OH).nH2O xerogel composite

International Nuclear Information System (INIS)

Zampronio, Elaine C.; Lassali, Tania A.F.; Oliveira, Herenilton P.

2005-01-01

In this work, we report the synthesis, characterization and electrochemical properties of a new multicomponent material obtained from the polymerization of vanadium pentoxide in an inorganic matrix (alumina xerogel), forming a xerogel composite. The material has been characterized by X-ray diffraction, infrared spectroscopy, thermogravimetric analysis, electron microscopy, energy dispersive X-ray spectrometry, cyclic voltammetry and impedance spectroscopy. It was found that the V 2 O 5 xerogel is dispersed in the alumina matrix, but its lamellar structure is not strongly affected, thus, its conductivity properties are maintained. Moreover, the electrochemical behaviour of the V 2 O 5 xerogel dispersed in the alumina matrix is quite similar to that found for the V 2 O 5 xerogel alone and the inorganic matrix leads to stabilization of V 2 O 5 xerogel structure

Controlled synthesis and electrochemical properties of vanadium ...

Indian Academy of Sciences (India)

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

Electrochemical potentials of layered oxide and olivine phosphate ...

Indian Academy of Sciences (India)

Lithium ion battery; cathodes; density functional theory; density of states; Bader charge analysis; electrochemical ... voltage, ionic diffusion coefficient, phase stability and charge ... routes to synthesis and fabrication techniques. .... from the lithiated one. ..... Ebner W, Fouchard D and Xie L 1994 Solid State Ionics 69 238.

Synthesis, characterization and electrochemical performance of Li 2 ...

Indian Academy of Sciences (India)

Positive electrodes; lithium metal silicates; electrical conductivity; cyclic performance ... Furthermore, electrochemical impedance spectra measurements are performed ... It was observed that Li–Li 2 Ni 0.4 Fe 0.6 SiO 4 battery has initial discharge ... Central Metallurgical Research and Development Institute (CMRDI), Tebbin, ...

Electrochemical co-reduction synthesis of graphene/nano-gold composites and its application to electrochemical glucose biosensor

International Nuclear Information System (INIS)

Wang, Xiaolin; Zhang, Xiaoli

2013-01-01

Graphical abstract: - Highlights: • Graphene/nano-Au composite was synthesized by electrochemical co-reduction method in one step. • Glucose oxidase achieves direct electrochemistry on the graphene/nano-Au composite film. • The glucose biosensor shows a high sensitivity of 56.93 μA mM −1 cm −2 toward glucose. • Glucose was detected with a wide linear range and low detection limit. - Abstract: A simple, green and controllable approach was employed for electrochemical synthesize of the graphene/nano-Au composites. The process was that graphene oxide and HAuCl 4 was electrochemically co-reduced onto the glassy carbon electrode (GCE) by cyclic voltammetry in one step. The obtained graphene/nano-Au/GCE exhibited high electrocatalytic activity toward H 2 O 2 , which resulted in a remarkable decrease in the overpotential of H 2 O 2 electrochemical oxidation compared with bare GCE. Such electrocatalytic behavior of the graphene/nano-Au/GCE permitted effective low-potential amperometric biosensing of glucose via the incorporation of glucose oxidase (GOD) with graphene/nano-Au. An obvious advantage of this enzyme electrode (graphene/nano-Au/GOD/GCE) was that the graphene/nano-Au nanocomposites provided a favorable microenvironment for GOD and facilitated the electron transfer between the active center of GOD and electrode. The immobilized GOD showed a direct, reversible redox reaction. Furthermore, the graphene/nano-Au/GOD/GCE was used as a glucose biosensor, displaying a low detection limit of 17 μM (S/N = 3), a high sensitivity of 56.93 μA mM −1 cm −2 , acceptable reproducibility, very good stability, selectivity and anti-interference ability

Electrochemical synthesis of poly(aniline-co-fluoroaniline) films and their application as humidity sensing material

International Nuclear Information System (INIS)

Sharma, Amit L.

2009-01-01

In the present manuscript, humidity sensing properties of a copolymer, poly(aniline-co-fluoroaniline) have been reported. The copolymer was prepared on indium-tin-oxide coated glass plates as well as platinum surface in the form of films using electrochemical technique (versus standard calomel electrode) in acidic medium. Synthesis of copolymer films was supported by Fourier transform infra-red, ultraviolet-visible, scanning electron microscope and cyclic voltammetry techniques. Molecular weight and electrical conductivity of these films were measured at different temperature. Polyaniline and poly(2-fluoroaniline) films were also synthesized using the same technique to compare the data with copolymer film. On exposure to humid atmosphere, the response behaviour of copolymer film exhibited a change in resistance with respect to relative humidity (RH). This copolymer film was found to be most sensitive in the 30-65% RH range and shows a linear behaviour with in this range.

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

International Nuclear Information System (INIS)

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

2005-01-01

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

Chromium(III) Complex Obtained from Dipicolinic Acid: Synthesis, Characterization, X-Ray Crystal Structure and Electrochemical Studies

Energy Technology Data Exchange (ETDEWEB)

Ghasemi, Khaled; Rezvani, Ali Reza; Ghasemi, Fatemeh [Univ. of Sistan and Baluchestan, Zahedan (Iran, Islamic Republic of); Razak, Ibrahim Abdul; Rosli, Mohd Mustaqim [Universiti Sains Malaysia, Penang (Malaysia)

2013-10-15

The synthesis, X-ray crystallography, spectroscopic (IR, UV-vis), and electrochemical properties of the title compound, [H{sub 3}O][Cr(dipic){sub 2}] [H{sub 3}O{sup +}.Cl{sup -}] (1), (H{sub 2}dipic = 2,6-pyridinedicarboxylic acid), are reported. This complex crystallizes in the monoclinic space group Cc with a = 14.9006(10) A, b = 12.2114(8) A, c = 8.6337(6) A, α = 90.00 .deg., β = 92.7460(10) .deg., γ = 90.00 .deg., and V = 1569.16(18) A3 with Z = 4. The hydrogen bonding and noncovalent interactions play roles in the stabilization of the structure. In order to gain a better understanding of the most important geometrical parameters in the structure of the complex, atoms in molecules (AIM) method at B3LYP/6-31G level of theory has been employed.

Synthesis and characterization of Nitrogen-doped &CaCO3-decorated reduced graphene oxide nanocomposite for electrochemical supercapacitors

International Nuclear Information System (INIS)

Ghouri, Zafar Khan; Barakat, Nasser A.M.; Alam, Al-Mahmnur; Alsoufi, Mohammad S.; Bawazeer, Tahani M.; Mohamed, Ahmed F.; Kim, Hak Yong

2015-01-01

Alone, it is expected, and also was experimentally proved, that calcium carbonate and reduced graphene oxide do have negligible specific capacitance due to the chemical composition of both materials. However, synthesis of CaCO 3 on the form of very thin sporadic layer attaching rGO results in dramatic increase in the specific capacitance of the obtained composite due to formation of the electrochemical double layer at the interfacial area. Moreover, the specific capacitance could be further enhanced by nitrogen-doping of the rGO sheets. Typically, a novel N-rGO/CaCO 3 composite has been successfully synthesized by heat reflux strategy with graphite powder, calcium acetate and urea as raw materials.The composite was characterized by X-Ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), field-emission scanning electron microscopy (FESEM), coupled with rapid EDAX (energy dispersive analysis of X-Ray) and X-ray photoelectron spectroscopy. The utilized physiochemical characterizations indicated that the final prepared composite can be demonstrated as N-doped rGO decorated by very thin discrete layer from calcium carbonate. Supercapacitive performance of N-rGO/CaCO 3 composite has been investigated by cyclic voltammetry (CV), galvanostatic charge-discharge and electrochemical impedance spectroscopy in 1 M KOH solution. The results reveal that the N-rGO/CaCO 3 composite delivers a large specific capacitance of as high as 214 Fg −1 and 188 Fg −1 at 5 mV s −1 and 1.0 Ag −1 , according to CV and galvanostatic charge-discharge tests, respectively; while the CaCO 3 , rGO, rGO/CaCO 3 , N-rGO based electrodes has a poor electrochemical performance at the same conditions. Moreover, the as-prepared composite exhibited excellent long cycle stability with about 88.7% specific capacitance retained after 10,000 cycles.

Synthesis and electrochemical study of Pt-based nanoporous materials

International Nuclear Information System (INIS)

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

2008-01-01

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

Synthesis and electrochemical study of Pt-based nanoporous materials

Energy Technology Data Exchange (ETDEWEB)

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

2008-10-01

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

Synthesis and electrochemical study of Pt-based nanoporous materials

Energy Technology Data Exchange (ETDEWEB)

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

2008-10-01

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

Electrochemical synthesis, in situ spectroelectrochemistry of conducting indole-titanium dioxide and zinc oxide polymer nanocomposites for rechargeable batteries

International Nuclear Information System (INIS)

Parvin, Mohammad Hadi; Pirnia, Mahsa; Arjomandi, Jalal

2015-01-01

Highlights: • Two novel hybrid materials-based conducting PIn rechargeable batteries were developed. • The charge-discharging behavior of PIn-nanocomposite batteries were studied. • The characterization of samples has been done by in situ spectroelectrochemical method. • PIn-TiO 2 and ZnO nanocomposites were synthesized electrochemically on Au and ITO. • The PIn-TiO 2 and ZnO nanocomposites resistances were less than PIn. - Abstract: Electrochemical synthesis, in situ spectroelectrochemistry of conducting polyindole (PIn), polyindole-TiO 2 (PIn-TiO 2 ) and polyindole-ZnO (PIn-ZnO) nanocomposites were investigated. The PIn and polymer nanocomposites were tested electrochemically for rechargeable batteries. The films were characterized by means of CVs, in situ UV-visible, FT-IR spectroscopies, in situ resistivity measurements, energy dispersive X-ray (EDX), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The charge-discharging behavior of a Zn/1 M ZnSO 4 /PIn cell with a capacity of around 90 Ah Kg −1 and on open circuit potential of around 1.45 V was compared with Zn/1 M ZnSO 4 /PIn-nanocomposite. The potential differences of redox couples (ΔE) for nanocomposites films show very good reversibility. A positive shift of potential was observed for polymer nanocomposites during redox scan. A significant variability was observed for in situ conductivity of the PIn and polymer nanocomposites. During in situ UV-visible and FT-IR measurements, intermediate spectroscopic behavior and positive shifts of wavelengths were observed for PIn and polymer nanocomposites. The SEM, TEM and EDX of nanocomposite films show the presence of nano particle in PIn.

Solvothermal Synthesis of Fe2O3 Loaded Activated Carbon as Electrode Materials for High-performance Electrochemical Capacitors

International Nuclear Information System (INIS)

Li, Ying; Kang, Litao; Bai, Gailing; Li, Peiyang; Deng, Jiachun; Liu, Xuguang; Yang, Yongzhen; Gao, Feng; Liang, Wei

2014-01-01

This article describes a facile solvothermal synthesis method to prepare Fe 2 O 3 /AC composites for electrochemical capacitors from Iron (III) chloride hexahydrate (FeCl 3 ·6H 2 O), activated carbon (AC, from petroleum coke), and four different precipitants (i.e., NaOH, CH 3 COONa, HMT, CO(NH 2 ) 2 ). X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), Energy dispersive spectroscopy (EDS) and Thermogravimetric (TG) analysis show that the products consisted of nanosized α-Fe 2 O 3 (weight ratios: 48.1, 47.9, 44.2, 44.3%) loaded onto AC particles (∼ 20 μm). Significantly, both kind and dosage of precipitants exhibit effects on the specific capacitances of Fe 2 O 3 /AC composites. The highest specific capacitance reaches up to 240 F g −1 (at a current density of 1 A g −1 in 6 M KOH aqueous electrolyte) when the molar ratio of CH 3 COONa: FeCl 3 is 9. On the other hand, the sample prepared with NaOH: FeCl 3 molar ratio being 1.5 exhibits excellent rate capability with specific capacitance of 215 F g −1 at 1 A g −1 , and 89.3, 82.3, 78.1, 72.6 and 65.1% capacity retention at 2, 5, 10, 20, and 40 A g −1 , respectively. These electrochemical performances are superior to other materials consisted of Fe 2 O 3 /carbon nanotube (CNT), graphene oxide (GO) or reduced graphene oxide (rGO) composites, demonstrating the great potential of Fe 2 O 3 /AC composites in the development of high-performance electrode materials for electrochemical capacitors

Synthesis and electrochemical properties of novel, donor–acceptor pyrrole derivatives with 1,8-naphthalimide units and their polymers

International Nuclear Information System (INIS)

Ledwon, Przemyslaw; Brzeczek, Alina; Pluczyk, Sandra; Jarosz, Tomasz; Kuznik, Wojciech; Walczak, Krzysztof; Lapkowski, Mieczyslaw

2014-01-01

A new class of bipolar monomers with pyrrole or thiophene–pyrrole–thiophene as electron donor and 1,8-naphthalimide as electron acceptor unit is reported. Donor–acceptor conjugated polymers were generated electrochemically. The synthesis of monomers, optical, electrochemical and spectroelectrochemical properties supported by theoretical calculations are presented. 1,8-naphthalimide units were attached directly to pyrrole in compounds 1a and 2a or by different bridges in the case of 1b and 2b. Intra-molecular donor–acceptor interactions of the monomers and its polymers were investigated using cyclic voltammetry, in-situ UV–Vis-NIR, electron spin resonance (ESR) spectroelectrochemistry and fluorescence spectroscopy. Studied compounds present large discrepancy (up to 1.31 eV for 2a) between energy gap values determined through electrochemical and optical measurements. The Time-dependent density functional theory (TDDFT) calculations help to explain this discrepancy. This is caused by weak HOMO to LUMO transition, 2000 times weaker than HOMO −2 to LUMO or HOMO to LUMO +1 transition. Altering the structure of monomers yields different stability and properties of obtained polymers. The p- and n-doping processes are separated. Anions are localized mainly on 1,8-naphthalimide units. Cations are localized mainly on pyrrole or thiophene–pyrrole–thiophene moiety and their polymer chains. Attachment of the additional thiophene units decreases the oxidation potential of the monomer and reduces the influence of the steric hindrance between 1,8-naphthalimide moiety and polymer/oligomers chain. This new class of model compounds is promising for use as a material with enhanced charge separation for wide range of optoelectronic, electrochromic and photovoltaic applications

Electrical and Electrochemical Properties of Conducting Polymers

Directory of Open Access Journals (Sweden)

Thanh-Hai Le

2017-04-01

Full Text Available Conducting polymers (CPs have received much attention in both fundamental and practical studies because they have electrical and electrochemical properties similar to those of both traditional semiconductors and metals. CPs possess excellent characteristics such as mild synthesis and processing conditions, chemical and structural diversity, tunable conductivity, and structural flexibility. Advances in nanotechnology have allowed the fabrication of versatile CP nanomaterials with improved performance for various applications including electronics, optoelectronics, sensors, and energy devices. The aim of this review is to explore the conductivity mechanisms and electrical and electrochemical properties of CPs and to discuss the factors that significantly affect these properties. The size and morphology of the materials are also discussed as key parameters that affect their major properties. Finally, the latest trends in research on electrochemical capacitors and sensors are introduced through an in-depth discussion of the most remarkable studies reported since 2003.

Synthesis of Ultra-Small Platinum, Palladium and Gold Nanoparticles by Shewanella loihica PV-4 Electrochemically Active Biofilm and Their Enhanced Catalytic Activities

KAUST Repository

Ahmed, Elaf

2018-02-21

Ultra-small nanoparticles (USNPs) of noble metals have a great potential in a variety of applications due to their high surface areas and high reactivity. This works employed electrochemically active biofilms (EABs) composed of a single bacterium strain of Shewanella loihica PV-4 and successfully synthesized USNPs of noble metal Au, Pd, and Pt. The synthesized USNPs had a size range between 2 and 7 nm and exhibited excellent catalytic performance in dye decomposition. The results of this work shine lights on the use of EABs in nanoparticle synthesis.

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

Energy Technology Data Exchange (ETDEWEB)

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

2006-05-15

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

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

Science.gov (United States)

Fedorov, Roman G; Mandler, Daniel

2013-02-28

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

Electrochemical synthesis and spectroscopic characterization of poly(N-phenylpyrrole coatings in an organic medium on iron and platinum electrodes

Directory of Open Access Journals (Sweden)

A.K.D. Diaw

2008-12-01

Full Text Available The electrochemical synthesis of poly(N-phenylpyrrole film was achieved on pretreated iron and platinum electrodes in acetonitrile solutions containing 0.1 M N-phenylpyrrole as the monomer and 0.1 M tetrabutylammonium trifluoromethane sulfonate (Bu4NCF3SO3 as the supporting-salt. The results showed that a surface treatment by 10 % aqueous nitric acid inhibits iron dissolution without preventing the N-phenylpyrrole oxidation. Very strongly adherent films were obtained at constant-potential, constant-current and cyclic voltammetry. XPS measurements, infrared (FT-IR and electronic absorption (UV-vis spectroscopies were used to characterize the iron and platinum-coated electrodes. Finally the anticorrosion properties of the PΦP film were evidenced.

Thermodynamic and achievable efficiencies for solar-driven electrochemical reduction of carbon dioxide to transportation fuels

Science.gov (United States)

Singh, Meenesh R.; Clark, Ezra L.; Bell, Alexis T.

2015-11-01

Thermodynamic, achievable, and realistic efficiency limits of solar-driven electrochemical conversion of water and carbon dioxide to fuels are investigated as functions of light-absorber composition and configuration, and catalyst composition. The maximum thermodynamic efficiency at 1-sun illumination for adiabatic electrochemical synthesis of various solar fuels is in the range of 32-42%. Single-, double-, and triple-junction light absorbers are found to be optimal for electrochemical load ranges of 0-0.9 V, 0.9-1.95 V, and 1.95-3.5 V, respectively. Achievable solar-to-fuel (STF) efficiencies are determined using ideal double- and triple-junction light absorbers and the electrochemical load curves for CO2 reduction on silver and copper cathodes, and water oxidation kinetics over iridium oxide. The maximum achievable STF efficiencies for synthesis gas (H2 and CO) and Hythane (H2 and CH4) are 18.4% and 20.3%, respectively. Whereas the realistic STF efficiency of photoelectrochemical cells (PECs) can be as low as 0.8%, tandem PECs and photovoltaic (PV)-electrolyzers can operate at 7.2% under identical operating conditions. We show that the composition and energy content of solar fuels can also be adjusted by tuning the band-gaps of triple-junction light absorbers and/or the ratio of catalyst-to-PV area, and that the synthesis of liquid products and C2H4 have high profitability indices.

Thermodynamic and achievable efficiencies for solar-driven electrochemical reduction of carbon dioxide to transportation fuels.

Science.gov (United States)

Singh, Meenesh R; Clark, Ezra L; Bell, Alexis T

2015-11-10

Thermodynamic, achievable, and realistic efficiency limits of solar-driven electrochemical conversion of water and carbon dioxide to fuels are investigated as functions of light-absorber composition and configuration, and catalyst composition. The maximum thermodynamic efficiency at 1-sun illumination for adiabatic electrochemical synthesis of various solar fuels is in the range of 32-42%. Single-, double-, and triple-junction light absorbers are found to be optimal for electrochemical load ranges of 0-0.9 V, 0.9-1.95 V, and 1.95-3.5 V, respectively. Achievable solar-to-fuel (STF) efficiencies are determined using ideal double- and triple-junction light absorbers and the electrochemical load curves for CO2 reduction on silver and copper cathodes, and water oxidation kinetics over iridium oxide. The maximum achievable STF efficiencies for synthesis gas (H2 and CO) and Hythane (H2 and CH4) are 18.4% and 20.3%, respectively. Whereas the realistic STF efficiency of photoelectrochemical cells (PECs) can be as low as 0.8%, tandem PECs and photovoltaic (PV)-electrolyzers can operate at 7.2% under identical operating conditions. We show that the composition and energy content of solar fuels can also be adjusted by tuning the band-gaps of triple-junction light absorbers and/or the ratio of catalyst-to-PV area, and that the synthesis of liquid products and C2H4 have high profitability indices.

Facile Synthesis of Flowerlike LiFe5O8 Microspheres for Electrochemical Supercapacitors.

Science.gov (United States)

Lin, Ying; Dong, Jingjing; Dai, Jingjing; Wang, Jingping; Yang, Haibo; Zong, Hanwen

2017-12-18

Facile synthesis of porous and hollow spinel materials is very urgent due to their extensive applications in the field of energy storage. In present work, flowerlike porous LiFe 5 O 8 microspheres etched for 15, 30, and 45 min (named as p-LFO-15, p-LFO-30, and p-LFO-45, respectively) are successfully synthesized through a facile chemical etching method based on bulk LiFe 5 O 8 (LFO) particles as precursors, and they are applied as electrode materials for high-performance electrochemical capacitors. In particular, the specific surface area of p-LFO-45 reaches 46.13 m 2 g -1 , which is 112 times greater than that of the unetched counterpart. Therefore, the p-LFO-45 electrode can achieve a higher capacitance of 278 F g -1 at a scan rate of 5 mV s -1 than the unetched counterpart. Furthermore, the p-LFO-45 electrode presents a good cycling stability with 78.3% of capacitive retention after 2000 cycles, which is much higher than that of the unetched LFO particles (66%). Therefore, the flowerlike porous LFO microspheres are very promising candidate materials for supercapacitor applications.

Synthesis, crystal structure and electrochemical properties of the manganese-doped LiNaFe[PO{sub 4}]F materials

Energy Technology Data Exchange (ETDEWEB)

Ben Yahia, Hamdi, E-mail: benyahia.hamdi@aist.go.jp; Shikano, Masahiro, E-mail: shikano.masahiro@aist.go.jp; Sakaebe, Hikari; Kobayashi, Hironori

2013-08-15

The new compounds LiNaFe{sub 1−x}Mn{sub x}[PO{sub 4}]F (x ≤ 1/4) were synthesized by a solid state reaction route. The crystal structure of LiNaFe{sub 3/4}Mn{sub 1/4}[PO{sub 4}]F was determined from single crystal X-ray diffraction data. LiNaFe{sub 3/4}Mn{sub 1/4}[PO{sub 4}]F crystallizes with the Li{sub 2}Ni[PO{sub 4}]F-type structure, space group Pnma, a = 10.9719(13), b = 6.3528(7), c = 11.4532(13) Å, V = 798.31(16) Å{sup 3}, and Z = 8. The structure consists of edge-sharing (Fe{sub 3/4}Mn{sub 1/4})O{sub 4}F{sub 2} octahedra forming (Fe{sub 3/4}Mn{sub 1/4})FO{sub 3} chains running along the b-axis. These chains are interlinked by PO{sub 4} tetrahedra forming a three-dimensional framework with the tunnels and the cavities filled by the well-ordered sodium and lithium atoms, respectively. The manganese-doped phases show poor electrochemical behavior comparing to the iron pure phase LiNaFe[PO{sub 4}]F. - Highlights: • We investigated the synthesis of LiNaFe{sub 1−x}Mn{sub x}[PO{sub 4}]F by solid state reaction. • We demonstrated that a solid solution exist only for x ≤ 1/4. • We solved the crystal structure of LiNaFe{sub 3/4}Mn{sub 1/4}[PO{sub 4}]F using single crystal data. • We studied the electrochemical performances of LiNaFe{sub 1−x}Mn{sub x}[PO{sub 4}]F. • The Mn-doped phases have poor electrochemical performances comparing to LiNaFe[PO{sub 4}]F.

The influence of the synthesis method of Ti/RuO2 electrodes on their stability and catalytic activity for electrochemical oxidation of the pesticide carbaryl

International Nuclear Information System (INIS)

Santos, T.É.S.; Silva, R.S.; Carlesi Jara, C.; Eguiluz, K.I.B.; Salazar-Banda, G.R.

2014-01-01

In this study, we developed dimensionally stable anodes of titanium covered with ruthenium oxides (Ti/RuO 2 ) using sol–gel, Pechini and ionic liquid (IL) methodologies. The electrochemical efficiency of these electrodes was then evaluated regarding electrochemical degradation of the pesticide carbaryl. The UV–visible spectroscopy measurements showed that the electrodes obtained by the IL and Pechini methods were more effective at pesticide degradation compared with the sol–gel electrode, especially at high current density values. Carbaryl degradation after 2 h of electrolysis at 30 mA cm −2 was 96.4% and 95.5% for the electrodes obtained by the IL and Pechini methods, respectively, while the degradation was 65.0% for the electrodes obtained by the sol–gel method. Additionally, the electrodes prepared by the IL and Pechini methods showed greater physical and electrochemical stability when compared to electrodes obtained by the sol–gel method. Electrodes prepared by the IL method with a few covering layers (three) achieved an elevated and constant area in a more efficient way than electrodes prepared by the Pechini and sol–gel methods. This fact can be attributed to the higher viscosity of the ionic liquid-based precursor solution, which transfers a higher amount of Ru in one single layer, compared to the other methods studied, thus reducing the time for synthesis, the number of calcination steps and the production costs of electrodes. - Highlights: • We developed dimensionally stable anodes containing ruthenium oxides. • Sol–gel, Pechini and ionic liquid methodologies were used. • The ionic liquid method covers the surfaces more efficiently and with few layers. • The proposed method reduces the time and production cost for synthesis of electrodes. • The electrodes synthesized present high stability and pesticide degradation activity

Synthesis and Photophysical Characterizations of Thermal -Stable Naphthalene Benzimidazoles

OpenAIRE

Erten Ela, Şule; Özçelik, Serdar; Eren, Ersin

2011-01-01

Microwave-assisted synthesis, photophysical and electrochemical properties of thermal-stable naphthalene benzimidazoles and naphthalimides are studied in this paper. Microwave-assisted synthesis of naphthalene benzimidazoles provide higher yields than the conventional thermal synthesis. Comparative photophysical properties of naphthalene benzimidazoles and naphthalimides are revealed that conjugation of electron-donating group onto naphthalimide moiety increases fluorescence ...

Electrochemical Synthesis, Structure Elucidation and Antibacterial Evaluation of 9a-aza-9a-chloro-9a-homoerythromycin A

Directory of Open Access Journals (Sweden)

Zoran Mandic

2014-09-01

Full Text Available Electrochemical synthesis, structure elucidation and antibacterial evaluation of 9a-aza-9a-chloro-9a-homoerythromycin A were carried out. It was found that the anodic oxidation of 9a-aza-9a-homoerythromycin A via electrogenerated reactive chlorine species leads to the chlorination of lactam nitrogen in high yield provided the pH of the reaction mixture is maintained above 3. NOESY spectra reveal the existence of the mixture of two conformational families in the solution, the "folding-out" conformer being slightly more abundant comparing to 9a-Aza-9a-homoerythromycin A. The chlorine substitution of lactam hydrogen resulted in improved antimicrobial potency against Sreptococcus pyogenes PSCB0542, Moraxella catarrhalis ATCC 25238, Haemophilus  influenzae ATCC 49247 and Enteroccocus faecalis ATCC 29212.

In situ synthesis of N and Cu functionalized mesoporous FDU-14 resins and carbons for electrochemical hydrogen storage

Energy Technology Data Exchange (ETDEWEB)

Kong, AiGuo; Wang, WenJuan; Yang, Fan; Ding, HanMing; Shan, YongKui [Department of Chemistry, East China Normal University, ShangHai 200062 (China)

2010-07-15

N and Cu cooperatively functionalized mesoporous resin and carbon materials with bicontinuous cubic structure (FDU-14) were obtained by a novel synthesis method. In this method, block copolymers were used as the templates as well as the precursors for the preparation of these modifying mesoporous materials. The CuC{sub 2}O{sub 4} in the channels of mesoporous FDU-14 resins was gotten by in situ oxidation of the templates in a catalytic redox system containing Cu{sup 2+}, Al{sup 3+}, NO{sub 3}{sup -}, PO{sub 4}{sup 3-}, SO{sub 4}{sup 2-} ions. Simultaneously, the phenol-formaldehyde resin frameworks were in situ functionalized by the amine group resulting from the reduction of NO{sub 3}{sup -}, leading to the formation of N and CuC{sub 2}O{sub 4} modified mesoporous FDU-14 resin materials. Its pyrolysis at the different temperatures resulted in the production of N and Cu cooperatively functionalized mesoporous FDU-14 resin and carbon materials. The structure and composition of these materials were characterized by the X-ray power diffraction, transmission electron microscopy, N{sub 2} adsorption-desorption analysis, X-ray photoelectron spectroscopy, infrared spectroscopy, thermogravimetry analysis, and inductive coupled plasma emission spectroscopy. The electrochemical measurement indicated that N and Cu cooperatively functionalized mesoporous FDU-14 carbon materials possessed the enhanced electrochemical hydrogen storage performance. (author)

High surface area synthesis, electrochemical activity, and stability of tungsten carbide supported Pt during oxygen reduction in proton exchange membrane fuel cells

Science.gov (United States)

Chhina, H.; Campbell, S.; Kesler, O.

The oxidation of carbon catalyst supports to carbon dioxide gas leads to degradation in catalyst performance over time in proton exchange membrane fuel cells (PEMFCs). The electrochemical stability of Pt supported on tungsten carbide has been evaluated on a carbon-based gas diffusion layer (GDL) at 80 °C and compared to that of HiSpec 4000™ Pt/Vulcan XC-72R in 0.5 M H 2SO 4. Due to other electrochemical processes occurring on the GDL, detailed studies were also performed on a gold mesh substrate. The oxygen reduction reaction (ORR) activity was measured both before and after accelerated oxidation cycles between +0.6 V and +1.8 V vs. RHE. Tafel plots show that the ORR activity remained high even after accelerated oxidation tests for Pt/tungsten carbide, while the ORR activity was extremely poor after accelerated oxidation tests for HiSpec 4000™. In order to make high surface area tungsten carbide, three synthesis routes were investigated. Magnetron sputtering of tungsten on carbon was found to be the most promising route, but needs further optimization.

High surface area synthesis, electrochemical activity, and stability of tungsten carbide supported Pt during oxygen reduction in proton exchange membrane fuel cells

Energy Technology Data Exchange (ETDEWEB)

Chhina, H. [Automotive fuel cell corporation, 9000 Glenlyon Parkway, Burnaby, BC (Canada); Department of Mechanical and Industrial Engineering, 5 King' s College Road, University of Toronto, Toronto, Ontario (Canada); Campbell, S. [Automotive fuel cell corporation, 9000 Glenlyon Parkway, Burnaby, BC (Canada); Kesler, O. [Department of Mechanical and Industrial Engineering, 5 King' s College Road, University of Toronto, Toronto, Ontario (Canada)

2008-04-15

The oxidation of carbon catalyst supports to carbon dioxide gas leads to degradation in catalyst performance over time in proton exchange membrane fuel cells (PEMFCs). The electrochemical stability of Pt supported on tungsten carbide has been evaluated on a carbon-based gas diffusion layer (GDL) at 80 C and compared to that of HiSpec 4000 trademark Pt/Vulcan XC-72R in 0.5 M H{sub 2}SO{sub 4}. Due to other electrochemical processes occurring on the GDL, detailed studies were also performed on a gold mesh substrate. The oxygen reduction reaction (ORR) activity was measured both before and after accelerated oxidation cycles between +0.6 V and +1.8 V vs. RHE. Tafel plots show that the ORR activity remained high even after accelerated oxidation tests for Pt/tungsten carbide, while the ORR activity was extremely poor after accelerated oxidation tests for HiSpec 4000 trademark. In order to make high surface area tungsten carbide, three synthesis routes were investigated. Magnetron sputtering of tungsten on carbon was found to be the most promising route, but needs further optimization. (author)

Fundamentals and applications of organic electrochemistry synthesis, materials, devices

CERN Document Server

Fuchigami, Toshio; Inagi, Shinsuke

2014-01-01

This textbook is an accessible overview of the broad field of organic electrochemistry, covering the fundamentals and applications of contemporary organic electrochemistry.  The book begins with an introduction to the fundamental aspects of electrode electron transfer and methods for the electrochemical measurement of organic molecules. It then goes on to discuss organic electrosynthesis of molecules and macromolecules, including detailed experimental information for the electrochemical synthesis of organic compounds and conducting polymers. Later chapters highlight new methodology for organic electrochemical synthesis, for example electrolysis in ionic liquids, the application to organic electronic devices such as solar cells and LEDs, and examples of commercialized organic electrode processes. Appendices present useful supplementary information including experimental examples of organic electrosynthesis, and tables of physical data (redox potentials of various organic solvents and organic compounds and phy...

Direct electrochemical imidation of aliphatic amines via anodic oxidation.

Science.gov (United States)

Zhang, Li; Su, Ji-Hu; Wang, Sujing; Wan, Changfeng; Zha, Zhenggen; Du, Jiangfeng; Wang, Zhiyong

2011-05-21

Direct electrochemical synthesis of sulfonyl amidines from aliphatic amines and sulfonyl azides was realized with good to excellent yields. Traditional tertiary amine substrates were broadened to secondary and primary amines. The reaction intermediates were observed and a reaction mechanism was proposed and discussed. © The Royal Society of Chemistry 2011

Synthesis and electrochemical characterization of hybrid membrane Nafion-SiO2 for application as polymer electrolyte in PEM fuel cell

International Nuclear Information System (INIS)

Dresch, Mauro Andre

2009-01-01

In this work, the effect of sol-gel synthesis parameters on the preparation and polarization response of Nafion-SiO 2 hybrids as electrolytes for proton exchange membrane fuel cells (PEMFC) operating at high temperatures (130 degree C) was evaluated. The inorganic phase was incorporated in a Nafion matrix with the following purposes: to improve the Nafion water uptake at high temperatures (> 100 degree C); to increase the mechanical strength of Nafion and; to accelerate the electrode reactions. The hybrids were prepared by an in-situ incorporation of silica into commercial Nafion membranes using an acid-catalyzed sol-gel route. The effects of synthesis parameters, such as catalyst concentration, sol-gel solvent, temperature and time of both hydrolysis and condensation reactions, and silicon precursor concentration (Tetraethyl orthosilicate - TEOS), were evaluated as a function on the incorporation degree and polarization response. Nafion-SiO 2 hybrids were characterized by gravimetry, thermogravimetric analysis (TGA), scanning electron microscopy and X-ray dispersive energy (SEM-EDS), electrochemical impedance spectroscopy (EIS), and X-ray small angle scattering (SAXS). The hybrids were tested as electrolyte in single H 2 /O 2 fuel cells in the temperature range of 80 - 130 degree C and at 130 degree C and reduced relative humidity (75% and 50%). Summarily, the hybrid performance showed to be strongly dependent on the synthesis parameters, mainly, the type of alcohol and the TEOS concentration. (author)

Thermodynamic and achievable efficiencies for solar-driven electrochemical reduction of carbon dioxide to transportation fuels

Science.gov (United States)

Singh, Meenesh R.; Clark, Ezra L.; Bell, Alexis T.

2015-01-01

Thermodynamic, achievable, and realistic efficiency limits of solar-driven electrochemical conversion of water and carbon dioxide to fuels are investigated as functions of light-absorber composition and configuration, and catalyst composition. The maximum thermodynamic efficiency at 1-sun illumination for adiabatic electrochemical synthesis of various solar fuels is in the range of 32–42%. Single-, double-, and triple-junction light absorbers are found to be optimal for electrochemical load ranges of 0–0.9 V, 0.9–1.95 V, and 1.95–3.5 V, respectively. Achievable solar-to-fuel (STF) efficiencies are determined using ideal double- and triple-junction light absorbers and the electrochemical load curves for CO2 reduction on silver and copper cathodes, and water oxidation kinetics over iridium oxide. The maximum achievable STF efficiencies for synthesis gas (H2 and CO) and Hythane (H2 and CH4) are 18.4% and 20.3%, respectively. Whereas the realistic STF efficiency of photoelectrochemical cells (PECs) can be as low as 0.8%, tandem PECs and photovoltaic (PV)-electrolyzers can operate at 7.2% under identical operating conditions. We show that the composition and energy content of solar fuels can also be adjusted by tuning the band-gaps of triple-junction light absorbers and/or the ratio of catalyst-to-PV area, and that the synthesis of liquid products and C2H4 have high profitability indices. PMID:26504215

Surfactant-assisted electrochemical deposition of {alpha}-cobalt hydroxide for supercapacitors

Energy Technology Data Exchange (ETDEWEB)

Zhao, Ting [School of Materials Science and Engineering, Nanyang Technological University, Singapore 639798 (Singapore); Jiang, Hao; Ma, Jan [School of Materials Science and Engineering, Nanyang Technological University, Singapore 639798 (Singapore); Temasek Laboratories, Nanyang Technological University, Singapore 637553 (Singapore)

2011-01-15

A N-methylpyrrolidone (NMP) assisted electrochemical deposition route has been developed to realize the synthesis of a dense {alpha}-Co(OH){sub 2} layered structure, which is composed of nanosheets, each with a thickness of 10 nm. The capacitive characteristics of the as-obtained {alpha}-Co(OH){sub 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 {alpha}-Co(OH){sub 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 {alpha}-Co(OH){sub 2} shows better electrochemical performance with specific capacitance of 651 F g{sup -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. (author)

The influence of the synthesis method of Ti/RuO{sub 2} electrodes on their stability and catalytic activity for electrochemical oxidation of the pesticide carbaryl

Energy Technology Data Exchange (ETDEWEB)

Santos, T. É.S. [Laboratório de Eletroquímica e Nanotecnologia, Instituto de Tecnologia e Pesquisa (ITP)/Programa de Pós-Graduação em Engenharia de Processos, Universidade Tiradentes, 49032–490 Aracaju, SE (Brazil); Silva, R. S. [Laboratório de Materiais Cerâmicos Avançados, Departamento de Física, Universidade Federal de Sergipe, 49.100-000 São Cristóvão, SE (Brazil); Carlesi Jara, C. [Escuela de Ingeniería Química, Pontificia Universidad Católica de Valparaíso, Av. Brasil No 2147, 2362804 Valparaíso (Chile); Eguiluz, K. I.B. [Laboratório de Eletroquímica e Nanotecnologia, Instituto de Tecnologia e Pesquisa (ITP)/Programa de Pós-Graduação em Engenharia de Processos, Universidade Tiradentes, 49032–490 Aracaju, SE (Brazil); Salazar-Banda, G.R., E-mail: gianrsb@gmail.com [Laboratório de Eletroquímica e Nanotecnologia, Instituto de Tecnologia e Pesquisa (ITP)/Programa de Pós-Graduação em Engenharia de Processos, Universidade Tiradentes, 49032–490 Aracaju, SE (Brazil)

2014-11-14

In this study, we developed dimensionally stable anodes of titanium covered with ruthenium oxides (Ti/RuO{sub 2}) using sol–gel, Pechini and ionic liquid (IL) methodologies. The electrochemical efficiency of these electrodes was then evaluated regarding electrochemical degradation of the pesticide carbaryl. The UV–visible spectroscopy measurements showed that the electrodes obtained by the IL and Pechini methods were more effective at pesticide degradation compared with the sol–gel electrode, especially at high current density values. Carbaryl degradation after 2 h of electrolysis at 30 mA cm{sup −2} was 96.4% and 95.5% for the electrodes obtained by the IL and Pechini methods, respectively, while the degradation was 65.0% for the electrodes obtained by the sol–gel method. Additionally, the electrodes prepared by the IL and Pechini methods showed greater physical and electrochemical stability when compared to electrodes obtained by the sol–gel method. Electrodes prepared by the IL method with a few covering layers (three) achieved an elevated and constant area in a more efficient way than electrodes prepared by the Pechini and sol–gel methods. This fact can be attributed to the higher viscosity of the ionic liquid-based precursor solution, which transfers a higher amount of Ru in one single layer, compared to the other methods studied, thus reducing the time for synthesis, the number of calcination steps and the production costs of electrodes. - Highlights: • We developed dimensionally stable anodes containing ruthenium oxides. • Sol–gel, Pechini and ionic liquid methodologies were used. • The ionic liquid method covers the surfaces more efficiently and with few layers. • The proposed method reduces the time and production cost for synthesis of electrodes. • The electrodes synthesized present high stability and pesticide degradation activity.

Use of Dendrimers during the Synthesis of Pt-Ru Electrocatalysts for PEM Fuel Cells: Effects on the Physical and Electrochemical Properties

Directory of Open Access Journals (Sweden)

J. C. Calderón

2011-01-01

Full Text Available In this work, Pt-Ru catalysts were synthesized by a novel methodology which includes the use as encapsulating molecules of dendrimers of different generation: zero (DN-0, one (DN-1, two (DN-2, and three (DN-3. Synthesized catalysts were heat-treated at 350°C, and the effects of this treatment was established from the physical (X-ray dispersive energy (XDE and X-ray diffraction (XRD and electrochemical characterization (cyclic voltammetry and chronoamperometry. Results showed that the heat-treatment benefits the catalytic properties of synthesized materials in terms of CO and methanol electrochemical oxidation. The curves for CO stripping were more defined for heat-treated catalysts, and methanol oxidation current densities were higher for these materials. These changes are principally explained from the removal of organic residues remaining on the surface of the Pt-Ru nanoparticles after the synthesis procedure. After the activation of the catalysts by heating at 350°C, the real importance of the use of these encapsulating molecules and the effect of the generation of the dendrimer become visible. From these results, it can be concluded that synthesized catalysts are good catalytic anodes for direct methanol fuel cells (DMFCs.

Manganese oxide-based materials as electrochemical supercapacitor electrodes.

Science.gov (United States)

Wei, Weifeng; Cui, Xinwei; Chen, Weixing; Ivey, Douglas G

2011-03-01

Electrochemical supercapacitors (ECs), characteristic of high power and reasonably high energy densities, have become a versatile solution to various emerging energy applications. This critical review describes some materials science aspects on manganese oxide-based materials for these applications, primarily including the strategic design and fabrication of these electrode materials. Nanostructurization, chemical modification and incorporation with high surface area, conductive nanoarchitectures are the three major strategies in the development of high-performance manganese oxide-based electrodes for EC applications. Numerous works reviewed herein have shown enhanced electrochemical performance in the manganese oxide-based electrode materials. However, many fundamental questions remain unanswered, particularly with respect to characterization and understanding of electron transfer and atomic transport of the electrochemical interface processes within the manganese oxide-based electrodes. In order to fully exploit the potential of manganese oxide-based electrode materials, an unambiguous appreciation of these basic questions and optimization of synthesis parameters and material properties are critical for the further development of EC devices (233 references).

Electrochemical Synthesis of Nitro-Chitosan and Its Performance in Chromium Removal

Directory of Open Access Journals (Sweden)

Scott M. McLennan

2013-07-01

Full Text Available A synthesized polymeric form of chitosan, electrochemically precipitated and photochemically modified, has been found to have significant value in removal of toxic chromate oxyanions from solution. Fourier Transform Infra-Red (FTIR, Raman and X-ray photoelectron spectroscopy (XPS indicated that a significant percentage of the amine functional groups were oxidized to nitro groups as a result of reactions with hydroxyl ions formed in the electrochemical process with additional oxidation occurring as a result of exposure to ultra-violet light. The adsorption capacity of the modified chitosan for chromate was investigated in a batch system by taking into account effects of initial concentration, pH of the solution and contact time. Nitro-chitosan showed greater adsorption capacity towards Cr (VI than other forms of chitosan, with a maximum adsorption of 173 mg/g. It was found that pH 3 is the optimum for adsorption, a Langmuir model is the best fit for the adsorption isotherm, and the kinetics of reaction followed a pseudo second order function. Overall, our results indicate that electrochemical modification of chitosan is an effective method to enhance the reactivity of chitosan towards metals.

Aerobic and Electrochemical Oxidations with N-Oxyl Reagents

Science.gov (United States)

Miles, Kelsey C.

Selective oxidation of organic compounds represents a significant challenge for chemical transformations. Oxidation methods that utilize nitroxyl catalysts have become increasingly attractive and include Cu/nitroxyl and nitroxyl/NO x co-catalyst systems. Electrochemical activation of nitroxyls is also well known and offers an appealing alternative to the use of chemical co-oxidants. However, academic and industrial organic synthetic communities have not widely adopted electrochemical methods. Nitroxyl catalysts facilitate effective and selective oxidation of alcohols and aldehydes to ketones and carboxylic acids. Selective benzylic, allylic, and alpha-heteroatom C-H abstraction can also be achieved with nitroxyls and provides access to oxygenated products when used in combination with molecular oxygen as a radical trap. This thesis reports various chemical and electrochemical oxidation methods that were developed using nitroxyl mediators. Chapter 1 provides a short review on practical aerobic alcohol oxidation with Cu/nitroxyl and nitroxyl/NO x systems and emphasizes the utility of bicyclic nitroxyls as co-catalysts. In Chapter 2, the combination of these bicyclic nitroxyls with NOx is explored for development of a mild oxidation of alpha-chiral aryl aldehydes and showcases a sequential asymmetric hydroformylation/oxidation method. Chapter 3 reports the synthesis and characterization of two novel Cu/bicyclic nitroxyl complexes and the electronic structure analysis of these complexes. Chapter 4 highlights the electrochemical activation of various nitroxyls and reports an in-depth study on electrochemical alcohol oxidation and compares the reactivity of nitroxyls under electrochemical or chemical activation. N-oxyls can also participate in selective C-H abstraction, and Chapter 5 reports the chemical and electrochemical activation of N-oxyls for radical-mediated C-H oxygenation of (hetero)arylmethanes. For these electrochemical transformations, the development of

Method and electrochemical cell for synthesis and treatment of metal monolayer electrocatalysts metal, carbon, and oxide nanoparticles ion batch, or in continuous fashion

Science.gov (United States)

Adzic, Radoslav; Zhang, Junliang; Sasaki, Kotaro

2015-04-28

An apparatus and method for synthesis and treatment of electrocatalyst particles in batch or continuous fashion is provided. In one embodiment, the apparatus comprises a sonication bath and a two-compartment chamber submerged in the sonication bath. The upper and lower compartments are separated by a microporous material surface. The upper compartment comprises a cover and a working electrode (WE) connected to a Pt foil contact, with the foil contact connected to the microporous material. The upper chamber further comprises reference counter electrodes. The lower compartment comprises an electrochemical cell containing a solution of metal ions. In one embodiment, the method for synthesis of electrocatalysts comprises introducing a plurality of particles into the apparatus and applying sonication and an electrical potential to the microporous material connected to the WE. After the non-noble metal ions are deposited onto the particles, the non-noble metal ions are displaced by noble-metal ions by galvanic displacement.

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

International Nuclear Information System (INIS)

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

2013-01-01

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

Thermodynamic and achievable efficiencies for solar-driven electrochemical reduction of carbon dioxide to transportation fuels

Energy Technology Data Exchange (ETDEWEB)

Singh, Meenesh R. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Joint Center for Artificial Photosynthesis, Material Science Division; Clark, Ezra L. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Joint Center for Artificial Photosynthesis, Material Science Division; Univ. of California, Berkeley, CA (United States). Dept. of Chemical & Biomolecular Engineering; Bell, Alexis T. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Joint Center for Artificial Photosynthesis, Material Science Division; Univ. of California, Berkeley, CA (United States). Dept. of Chemical & Biomolecular Engineering

2015-10-26

Thermodynamic, achievable, and realistic efficiency limits of solar-driven electrochemical conversion of water and carbon dioxide to fuels are investigated as functions of light-absorber composition and configuration, and catalyst composition. The maximum thermodynamic efficiency at 1-sun illumination for adiabatic electrochemical synthesis of various solar fuels is in the range of 32–42%. Single-, double-, and triple-junction light absorbers are found to be optimal for electrochemical load ranges of 0–0.9 V, 0.9–1.95 V, and 1.95–3.5 V, respectively. Achievable solar-to-fuel (STF) efficiencies are determined using ideal double- and triple-junction light absorbers and the electrochemical load curves for CO₂ reduction on silver and copper cathodes, and water oxidation kinetics over iridium oxide. The maximum achievable STF efficiencies for synthesis gas (H₂ and CO) and Hythane (H₂ and CH₄) are 18.4% and 20.3%, respectively. Whereas the realistic STF efficiency of photoelectrochemical cells (PECs) can be as low as 0.8%, tandem PECs and photovoltaic (PV)-electrolyzers can operate at 7.2% under identical operating conditions. Finally, we show that the composition and energy content of solar fuels can also be adjusted by tuning the band-gaps of triple-junction light absorbers and/or the ratio of catalyst-to-PV area, and that the synthesis of liquid products and C₂H₄ have high profitability indices.

Self-template synthesis of double shelled ZnS-NiS1.97 hollow spheres for electrochemical energy storage

Science.gov (United States)

Wei, Chengzhen; Ru, Qinglong; Kang, Xiaoting; Hou, Haiyan; Cheng, Cheng; Zhang, Daojun

2018-03-01

In this work, double shelled ZnS-NiS1.97 hollow spheres have been achieved via a simple self-template route, which involves the synthesis of Zn-Ni solid spheres precursors as the self-template and then transformation into double shelled ZnS-NiS1.97 hollow spheres by sulfidation treatment. The as-prepared double shelled ZnS-NiS1.97 hollow spheres possess a high surface area (105.26 m2 g-1) and porous structures. Benefiting from the combined characteristics of novel structures, multi-component, high surface area and porous. When applied as electrode materials for supercapacitors, the double shelled ZnS-NiS1.97hollow spheres deliver a large specific capacitance of 696.8C g-1 at 5.0 A g-1 and a remarkable long lifespan cycling stability (less 5.5% loss after 6000 cycles). Moreover, an asymmetric supercapacitor (ASC) was assembled by utilizing ZnS-NiS1.97 (positive electrode) and activated carbon (negative electrode) as electrode materials. The as-assembled device possesses an energy density of 36 W h kg-1, which can be yet retained 25.6 W h kg-1 even at a power density of 2173.8 W Kg-1, indicating its promising applications in electrochemical energy storage. More importantly, the self-template route is a simple and versatile strategy for the preparation of metal sulfides electrode materials with desired structures, chemical compositions and electrochemical performances.

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

International Nuclear Information System (INIS)

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

2013-01-01

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

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

KAUST Repository

Rangaswamy, Puttaswamy

2016-10-13

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

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

KAUST Repository

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

2016-01-01

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

Synthesis of graphene nanomaterials and their application in electrochemical energy storage

Science.gov (United States)

Xiong, Guoping

The need to store and use energy on diverse scales in a modern technological society necessitates the design of large and small energy systems, among which electrical energy storage systems such as batteries and capacitors have attracted much interest in the past several decades. Supercapacitors, also known as ultracapacitors, or electrochemical capacitors, with fast power delivery and long cycle life are complementing or even replacing batteries in many applications. The rapid development of miniaturized electronic devices has led to a growing need for rechargeable micro-power sources with high performance. Among different sources, electrochemical micro-capacitors or micro-supercapacitors provide higher power density than their counterparts and are gaining increased interest from the research and engineering communities. Rechargeable Li ion batteries with high energy and power density, long cycling life, high charge-discharge rate (1C - 3C) and safe operation are in high demand as power sources and power backup for hybrid electric vehicles and other applications. In the present work, graphene-based graphene materials have been designed and synthesized for electrochemical energy storage applications, e.g., conventional supercapacitors (macro-supercapacitors), microsupercapacitors and lithium ion batteries. Factors influencing the formation and structure of graphitic petals grown by microwave plasma-enhanced chemical vapor deposition on oxidized silicon substrates were investigated through process variation and materials analysis. Insights gained into the growth mechanism of these graphitic petals suggest a simple scribing method can be used to control both the location and formation of petals on flat Si substrates. Transitional metal oxides and conducting polymers have been coated on the graphitic petal-based electrodes by facile chemical methods for multifunctional energy storage applications. Detailed electrochemical characterization (e.g., cyclic voltammetry and

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

Science.gov (United States)

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

2016-05-01

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

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

Science.gov (United States)

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

International Nuclear Information System (INIS)

Zhao, Jiangshan; Zhang, Qiang

2015-01-01

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

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

International Nuclear Information System (INIS)

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

2017-01-01

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

Lanthanide(III) complexes of bis-semicarbazone and bis-imine-substituted phenanthroline ligands: solid-state structures, photophysical properties, and anion sensing.

Science.gov (United States)

Nadella, Sandeep; Selvakumar, Paulraj M; Suresh, Eringathodi; Subramanian, Palani S; Albrecht, Markus; Giese, Michael; Fröhlich, Roland

2012-12-21

Phenanthroline-based hexadentate ligands L(1) and L(2) bearing two achiral semicarbazone or two chiral imine moieties as well as the respective mononuclear complexes incorporating various lanthanide ions, such as La(III), Eu(III), Tb(III), Lu(III), and Y(III) metal ions, were synthesized, and the crystal structures of [ML(1)Cl(3)] (M=La(III), Eu(III), Tb(III), Lu(III), or Y(III)) complexes were determined. Solvent or water molecules act as coligands for the rare-earth metals in addition to halide anions. The big Ln(III) ion exhibits a coordination number (CN) of 10, whereas the corresponding Eu(III), Tb(III), Lu(III), and Y(III) centers with smaller ionic radii show CN=9. Complexes of L(2), namely [ML(2)Cl(3)] (M=Eu(III), Tb(III), Lu(III), or Y(III)) ions could also be prepared. Only the complex of Eu(III) showed red luminescence, whereas all the others were nonluminescent. The emission properties of the Eu derivative can be applied as a photophysical signal for sensing various anions. The addition of phosphate anions leads to a unique change in the luminescence behavior. As a case study, the quenching behavior of adenosine-5'-triphosphate (ATP) was investigated at physiological pH value in an aqueous solvent. A specificity of the sensor for ATP relative to adenosine-5'-diphosphate (ADP) and adenosine-5'-monophosphate (AMP) was found. (31)P NMR spectroscopic studies revealed the formation of a [EuL(2)(ATP)] coordination species. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Supporting Information Synthesis Procedure: Graphene oxide (GO ...

Indian Academy of Sciences (India)

SS

Synthesis Procedure: Graphene oxide (GO) was prepared by a modified Hummers method using expandable .... anode material for Li ion batteries, J. Solid State Electrochem. ... coupling, doping and nonadiabatic effects, Solid State Commun.

Controllable synthesis and electrochemical hydrogen storage properties of Sb₂Se₃ ultralong nanobelts with urchin-like structures.

Science.gov (United States)

Jin, Rencheng; Chen, Gang; Pei, Jian; Sun, Jingxue; Wang, Yang

2011-09-01

The controlled synthesis of one-dimensional and three-dimensional Sb(2)Se(3) nanostructures has been achieved by a facile solvothermal process in the presence of citric acid. By simply controlling the concentration of citric acid, the nucleation, growth direction and exposed facet can be readily tuned, which brings the different morphologies and nanostructures to the final products. The as-prepared products have been characterized by means of X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy (TEM), high-resolution TEM and selected area electron diffraction. Based on the electron microscope observations, a possible growth mechanism of Sb(2)Se(3) with distinctive morphologies including ultralong nanobelts, hierarchical urchin-like nanostructures is proposed and discussed in detail. The electrochemical hydrogen storage measurements reveal that the morphology plays a key role on the hydrogen storage capacity of Sb(2)Se(3) nanostructures. The Sb(2)Se(3) ultralong nanobelts with high percentage of {-111} facets exhibit higher hydrogen storage capacity (228.5 mA h g(-1)) and better cycle stability at room temperature.

In situ self-sacrificed template synthesis of vanadium nitride/nitrogen-doped graphene nanocomposites for electrochemical capacitors.

Science.gov (United States)

Liu, Hong-Hui; Zhang, Hong-Ling; Xu, Hong-Bin; Lou, Tai-Ping; Sui, Zhi-Tong; Zhang, Yi

2018-03-15

Vanadium nitride and graphene have been widely used as pseudo-capacitive and electric double-layer capacitor electrode materials for electrochemical capacitors, respectively. However, the poor cycling stability of vanadium nitride and the low capacitance of graphene impeded their practical applications. Herein, we demonstrated an in situ self-sacrificed template method for the synthesis of vanadium nitride/nitrogen-doped graphene (VN/NGr) nanocomposites by the pyrolysis of a mixture of dicyandiamide, glucose, and NH 4 VO 3 . Vanadium nitride nanoparticles of the size in the range of 2 to 7 nm were uniformly embedded into the nitrogen-doped graphene skeleton. Furthermore, the VN/NGr nanocomposites with a high specific surface area and pore volume showed a high specific capacitance of 255 F g -1 at 10 mV s -1 , and an excellent cycling stability (94% capacitance retention after 2000 cycles). The excellent capacitive properties were ascribed to the excellent conductivity of nitrogen-doped graphene, high surface area, high pore volume, and the synergistic effect between vanadium nitride and nitrogen-doped graphene.

EDTA assisted synthesis of hydroxyapatite nanoparticles for electrochemical sensing of uric acid.

Science.gov (United States)

Kanchana, P; Sekar, C

2014-09-01

Hydroxyapatite nanoparticles have been synthesized using EDTA as organic modifier by a simple microwave irradiation method and its application for the selective determination of uric acid (UA) has been demonstrated. Electrochemical behavior of uric acid at HA nanoparticle modified glassy carbon electrode (E-HA/GCE) has been investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), linear sweep voltammetry (LSV) and amperometry. The E-HA modified electrode exhibits efficient electrochemical activity towards uric acid sensing without requiring enzyme or electron mediator. Amperometry studies revealed that the fabricated electrode has excellent sensitivity for uric acid with the lowest detection limit of 142 nM over a wide concentration range from 1 × 10(-7) to 3 × 10(-5)M. Moreover, the studied E-HA modified GC electrode exhibits a good reproducibility and long-term stability and an admirable selectivity towards the determination of UA even in the presence of potential interferents. The analytical performance of this sensor was evaluated for the detection of uric acid in human urine and blood serum samples. Copyright © 2014. Published by Elsevier B.V.

Electrochemical Deposition of Conformal and Functional Layers on High Aspect Ratio Silicon Micro/Nanowires.

Science.gov (United States)

Ozel, Tuncay; Zhang, Benjamin A; Gao, Ruixuan; Day, Robert W; Lieber, Charles M; Nocera, Daniel G

2017-07-12

Development of new synthetic methods for the modification of nanostructures has accelerated materials design advances to furnish complex architectures. Structures based on one-dimensional (1D) silicon (Si) structures synthesized using top-down and bottom-up methods are especially prominent for diverse applications in chemistry, physics, and medicine. Yet further elaboration of these structures with distinct metal-based and polymeric materials, which could open up new opportunities, has been difficult. We present a general electrochemical method for the deposition of conformal layers of various materials onto high aspect ratio Si micro- and nanowire arrays. The electrochemical deposition of a library of coaxial layers comprising metals, metal oxides, and organic/inorganic semiconductors demonstrate the materials generality of the synthesis technique. Depositions may be performed on wire arrays with varying diameter (70 nm to 4 μm), pitch (5 μ to 15 μ), aspect ratio (4:1 to 75:1), shape (cylindrical, conical, hourglass), resistivity (0.001-0.01 to 1-10 ohm/cm 2 ), and substrate orientation. Anisotropic physical etching of wires with one or more coaxial shells yields 1D structures with exposed tips that can be further site-specifically modified by an electrochemical deposition approach. The electrochemical deposition methodology described herein features a wafer-scale synthesis platform for the preparation of multifunctional nanoscale devices based on a 1D Si substrate.

Asymmetric synthesis using chiral-encoded metal

Science.gov (United States)

Yutthalekha, Thittaya; Wattanakit, Chularat; Lapeyre, Veronique; Nokbin, Somkiat; Warakulwit, Chompunuch; Limtrakul, Jumras; Kuhn, Alexander

2016-08-01

The synthesis of chiral compounds is of crucial importance in many areas of society and science, including medicine, biology, chemistry, biotechnology and agriculture. Thus, there is a fundamental interest in developing new approaches for the selective production of enantiomers. Here we report the use of mesoporous metal structures with encoded geometric chiral information for inducing asymmetry in the electrochemical synthesis of mandelic acid as a model molecule. The chiral-encoded mesoporous metal, obtained by the electrochemical reduction of platinum salts in the presence of a liquid crystal phase and the chiral template molecule, perfectly retains the chiral information after removal of the template. Starting from a prochiral compound we demonstrate enantiomeric excess of the (R)-enantiomer when using (R)-imprinted electrodes and vice versa for the (S)-imprinted ones. Moreover, changing the amount of chiral cavities in the material allows tuning the enantioselectivity.

Synthesis of Bi2WO6 nanoparticles and its electrochemical properties in different electrolytes for pseudocapacitor electrodes

International Nuclear Information System (INIS)

Nithya, V.D.; Kalai Selvan, R.; Kalpana, D.; Vasylechko, Leonid; Sanjeeviraja, C.

2013-01-01

Highlights: • A simple, economical and environmentally benign sonochemical technique was utilized for the synthesis of homogeneous Bi 2 WO 6 nanoparticles. • This is the first attempt to employ Bi 2 WO 6 as a supercapacitor electrode material. • Effect of electrolyte on the capacitive behaviour of the material is studied. • Bi 2 WO 6 displays good capacitive behaviour in 1 M KOH compared with 1 M NaOH and 1 M LiOH and possess sufficient capacity retention. • It presented an energy density of 67 Wh/kg in the potential range from −0.9 V to 0.1 V and it would be a promising negative electrode for supercapacitor. -- Abstract: Nanosized Bi 2 WO 6 particles were successfully synthesized by sonochemical method with an objective to develop an inexpensive and eco-friendly electrode material for supercapacitors. The prepared material was subjected to various thermal, structural, morphological, compositional, electrical and electrochemical studies. Bi 2 WO 6 nanoparticle with homogeneous distribution was achieved through sonochemical process. The lattice parameter and atomic positions of Bi 2 WO 6 structure were refined through Reitveld analysis. The electrochemical performance of Bi 2 WO 6 nanoparticles was investigated in various aqueous electrolytes such as 1 M NaOH, 1 M LiOH, 1 M Na 2 SO 4 , 1 M KOH and 6 M KOH solutions. Among these, the material exhibited an enhanced electrochemical performance in KOH electrolyte due to its smaller hydration sphere radius, high ionic mobility and lower equivalent series resistance. The charge–discharge studies rendered a specific capacitance of 608 F/g in 1 M KOH at a current density of 0.5 mA/cm 2 . Bi 2 WO 6 exhibited an excellent coulombic efficiency and specific capacitance of around 304 F/g at 3 mA/cm 2 in the potential range from −0.9 to 0.1 V vs Hg/HgO in 1 M KOH electrolyte. The above results assured that Bi 2 WO 6 could be utilized as suitable negative electrode material for supercapacitor applications and 1 M

Synthesis of LiFePO4/Graphene Nano composite and Its Electrochemical Properties as Cathode Material for Li-Ion Batteries

International Nuclear Information System (INIS)

Ma, X.; Chen, G.; Liu, Q.; Zeng, G.; Wu, T.

2014-01-01

LiFePO 4 /graphene nano composite was successfully synthesized by rheological phase method and its electrochemical properties as the cathode materials for lithium ion batteries were measured. As the iron source in the synthesis, FeOOH nano rods anchored on graphene were first synthesized. The FeOOH nano rods precursors and the final LiFePO 4 /graphene nano composite products were characterized by XRD, SEM, and TEM. While the FeOOH precursors were nano rods with 5-10 nm in diameter and 10-50 nm in length, the LiFePO 4 were nanoparticles with 20-100 nm in size. Compared with the electrochemical properties of LiFePO 4 particles without graphene nano sheets, it is clear that the graphene nano sheets can improve the performances of LiFePO 4 as the cathode material for lithium ion batteries. The as-synthesized LiFePO 4 /graphene nano composite showed high capacities and good cyclabilities. When measured at room temperature and at the rate of 0.1 C (1 C = 170 mA g -1 ), the composite showed a discharge capacity of 156 mA h g -1 in the first cycle and a capacity retention of 96% after 15 cycles. The improved performances of the composite are believed to be the result of the three-dimensional conducting network formed by the flexible and planar graphene nano sheets.

Synthesis and electrochemical characterization of mesoporous Li2FeSiO4/C composite cathode material for Li-ion batteries

Science.gov (United States)

Kumar, Ajay; Jayakumar, O. D.; Bazzi, Khadije; Nazri, Gholam-Abbas; Naik, Vaman M.; Naik, Ratna

2015-03-01

Lithium iron silicate (Li2FeSiO4) has the potential as cathode for Li ion batteries due to its high theoretical capacity (~ 330 mAh/g) and improved safety. The application of Li2FeSiO4 as cathode material has been challenged by its poor electronic conductivity and slow lithium ion diffusion in the solid phase. In order to solve these problems, we have synthesized mesoporous Li2FeSiO4/C composites by sol-gel method using the tri-block copolymer (P123) as carbon source. The phase purity and morphology of the composite materials were characterized by x-ray diffraction, SEM and TEM. The XRD pattern confirmed the formation of ~ 12 nm size Li2FeSiO4 crystallites in composites annealed at 600 °C for 6 h under argon atmosphere. The electrochemical properties are measured using the composite material as positive electrode in a standard coin cell configuration with lithium as the active anode and the cells were tested using AC impedance spectroscopy, cyclic voltammetry, and galvanostatic charge/discharge cycling. The Li2FeSiO4/C composites showed a discharge capacity of ~ 240 mAh/g at a rate of C/30 at room temperature. The effect of different annealing temperature and synthesis time on the electrochemical performance of Li2FeSiO4/C will be presented.

Freeze drying synthesis of Li{sub 3}MnO{sub 4} cathode material for Li-ion batteries: A physico-electrochemical study

Energy Technology Data Exchange (ETDEWEB)

Surace, Yuri; Simões, Mário; Karvonen, Lassi; Yoon, Songhak; Pokrant, Simone [Laboratory Materials for Energy Conversion, EMPA – Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Weidenkaff, Anke, E-mail: weidenkaff@imw.uni-stuttgart.de [Materials Chemistry, Institute for Materials Science, University of Stuttgart, Heisenbergstrasse 3, DE-70569 Stuttgart (Germany)

2015-09-25

Highlights: • Facilitated synthesis of Li{sub 3}MnO{sub 4} with a smaller thermal budget via freeze drying. • Electrochemical activity enhanced by micro- and nanostructure modifications. • Capacity increase of 30% at 1st discharge versus standard synthesis process. - Abstract: Li{sub 3}MnO{sub 4}, a lithium rich phase containing manganese (V), is a promising cathode material for Li-ion batteries due to its very high theoretical capacity (698 A h kg{sup −1}). Li{sub 3}MnO{sub 4} was synthesized from freeze dried precursors at 398 K. Combined structural, morphological and chemical characterization by XRD, TGA, SEM, TEM and XPS revealed improvements in the micro- and nanostructure in comparison to the material synthesized by a standard solid state chemistry route. The average particle size decreased from 10 μm to 3.5 μm and the average crystallite size from close to 100 nm to around 30 nm. These modifications enhanced the capacity (23% at 10 A kg{sup −1} and up to 31% at 50 A kg{sup −1} with a maximum discharge capacity of 290 A h kg{sup −1}) and the rate capability.

Synthesis of LiFePO4/Graphene Nanocomposite and Its Electrochemical Properties as Cathode Material for Li-Ion Batteries

Directory of Open Access Journals (Sweden)

Xiaoling Ma

2015-01-01

Full Text Available LiFePO4/graphene nanocomposite was successfully synthesized by rheological phase method and its electrochemical properties as the cathode materials for lithium ion batteries were measured. As the iron source in the synthesis, FeOOH nanorods anchored on graphene were first synthesized. The FeOOH nanorods precursors and the final LiFePO4/graphene nanocomposite products were characterized by XRD, SEM, and TEM. While the FeOOH precursors were nanorods with 5–10 nm in diameter and 10–50 nm in length, the LiFePO4 were nanoparticles with 20–100 nm in size. Compared with the electrochemical properties of LiFePO4 particles without graphene nanosheets, it is clear that the graphene nanosheets can improve the performances of LiFePO4 as the cathode material for lithium ion batteries. The as-synthesized LiFePO4/graphene nanocomposite showed high capacities and good cyclabilities. When measured at room temperature and at the rate of 0.1C (1C = 170 mA g−1, the composite showed a discharge capacity of 156 mA h g−1 in the first cycle and a capacity retention of 96% after 15 cycles. The improved performances of the composite are believed to be the result of the three-dimensional conducting network formed by the flexible and planar graphene nanosheets.

High-performance symmetric electrochemical capacitor based on graphene foam and nanostructured manganese oxide

CSIR Research Space (South Africa)

Bello, A

2013-01-01

Full Text Available We have fabricated a symmetric electrochemical capacitor with high energy and power densities based on a composite of graphene foam (GF) with 80 wt% of manganese oxide (MnO(sub2)) deposited by hydrothermal synthesis. Raman spectroscopy and X...

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

International Nuclear Information System (INIS)

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

2014-01-01

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

JV Task-121 Electrochemical Synthesis of Nitrogen Fertilizers

Energy Technology Data Exchange (ETDEWEB)

Junhua Jiang; Ted Aulich

2008-11-30

An electrolytic renewable nitrogen fertilizer process that utilizes wind-generated electricity, N{sub 2} extracted from air, and syngas produced via the gasification of biomass to produce nitrogen fertilizer ammonia was developed at the University of North Dakota Energy & Environmental Research Center. This novel process provides an important way to directly utilize biosyngas generated mainly via the biomass gasification in place of the high-purity hydrogen which is required for Haber Bosch-based production of the fertilizer for the production of the widely used nitrogen fertilizers. Our preliminary economic projection shows that the economic competitiveness of the electrochemical nitrogen fertilizer process strongly depends upon the cost of hydrogen gas and the cost of electricity. It is therefore expected the cost of nitrogen fertilizer production could be considerably decreased owing to the direct use of cost-effective 'hydrogen-equivalent' biosyngas compared to the high-purity hydrogen. The technical feasibility of the electrolytic process has been proven via studying ammonia production using humidified carbon monoxide as the hydrogen-equivalent vs. the high-purity hydrogen. Process optimization efforts have been focused on the development of catalysts for ammonia formation, electrolytic membrane systems, and membrane-electrode assemblies. The status of the electrochemical ammonia process is characterized by a current efficiency of 43% using humidified carbon monoxide as a feedstock to the anode chamber and a current efficiency of 56% using high-purity hydrogen as the anode gas feedstock. Further optimization of the electrolytic process for higher current efficiency and decreased energy consumption is ongoing at the EERC.

Nanocrystalline CdTe thin films by electrochemical synthesis

Directory of Open Access Journals (Sweden)

Ramesh S. Kapadnis

2013-03-01

Full Text Available Cadmium telluride thin films were deposited onto different substrates as copper, Fluorine-doped tin oxide (FTO, Indium tin oxide (ITO, Aluminum and zinc at room temperature via electrochemical route. The morphology of the film shows the nanostructures on the deposited surface of the films and their growth in vertical direction. Different nanostructures developed on different substrates. The X-ray diffraction study reveals that the deposited films are nanocrystalline in nature. UV-Visible absorption spectrum shows the wide range of absorption in the visible region. Energy-dispersive spectroscopy confirms the formation of cadmium telluride.

Synthesis, structure and electrochemical properties of polyaniline/MoO3 nanobelt composite for lithium battery

International Nuclear Information System (INIS)

Mohan, Varishetty Madhu; Chen, Wen; Murakami, Kenji

2013-01-01

Graphical abstract: Hydrothermal method was introduced for the synthesis of MoO 3 nanobelts and polyaniline (PANI)/MoO 3 nanobelt composites. The structure and morphology of the samples were studied by X-ray diffraction (XRD), Fourier transform infrared radiation (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analysis. We can see the presence of polyaniline on the MoO 3 nanobelts surface in the TEM pictures as shown in Fig. (a). The pure MoO 3 nanobelts exhibit the initial specific capacity 276 mAhg −1 , whereas PANI/MoO 3 nanobelt composite shows little low initially 228 mAhg −1 after that it has more stabilized specific capacity with increasing cycle numbers as shown in Fig. (b). The cyclic voltammograms of the PANI/MoO 3 nanobelt composite show better cyclic performance compared to pure MoO 3 nanobelts. The electrochemical impedance spectres were studied for both the pure and PANI/MoO 3 samples at 2.0 and 3.5 potentials. The role of the PANI polymeric component of the composite material seems to be the stabilization of the specific capacity due to probable homogeneous distribution of the induced stress during cycling. Display Omitted Highlights: ► Hydrothermal synthesis of MoO 3 , PANI/MoO 3 nanobelts. ► Samples were characterised by XRD, FTIR, DSC, SEM, TEM, CV and impedance. ► MoO 3 nanobelts cathode battery shows initial specific capacity 276 mAhg −1 . ► PANI/MoO 3 nanobelts show initial specific capacity 228 mAhg −1 but high stability. ► PANI/MoO 3 sample studies by impedance at the potentials of 2.0 and 3.5 V. -- Abstract: The MoO 3 nanobelts and polyaniline (PANI)/MoO 3 nanobelt composite were synthesized using hydrothermal method. The crystal structure and morphology of the samples were studied by X-ray diffraction (XRD), Fourier transform infrared radiation (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Differential scanning calorimetric (DSC) and thermo

Hydrothermal-reduction synthesis of manganese oxide nanomaterials for electrochemical supercapacitors.

Science.gov (United States)

Zhang, Xiong; Chen, Yao; Yu, Peng; Ma, Yanwei

2010-11-01

In the present work, amorphous manganese oxide nanomaterials have been synthesized by a common hydrothermal method based on the redox reaction between MnO4(-) and Fe(2+) under an acidic condition. The synthesized MnO2 samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and electrochemical studies. XRD results showed that amorphous manganese oxide phase was obtained. XPS quantitative analysis revealed that the atomic ratio of Mn to Fe was 3.5 in the MnO2 samples. TEM images showed the porous structure of the samples. Electrochemical properties of the MnO2 electrodes were studied using cyclic voltammetry and galvanostatic charge-discharge cycling in 1 M Na2SO4 aqueous electrolyte, which showed excellent pseudocapacitance properties. A specific capacitance of 192 Fg(-1) at a current density of 0.5 Ag(-1) was obtained at the potential window from -0.1 to 0.9 V (vs. SCE).

Recent Advances in Porous Carbon Materials for Electrochemical Energy Storage.

Science.gov (United States)

Wang, Libin; Hu, Xianluo

2018-06-18

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

Synthesis and Thermophysical Properties of Ether-Functionalized Sulfonium Ionic Liquids as Potential Electrolytes for Electrochemical Applications.

Science.gov (United States)

Coadou, Erwan; Goodrich, Peter; Neale, Alex R; Timperman, Laure; Hardacre, Christopher; Jacquemin, Johan; Anouti, Mérièm

2016-12-05

During this work, a novel series of hydrophobic room temperature ionic liquids (ILs) based on five ether functionalized sulfonium cations bearing the bis{(trifluoromethyl)sulfonyl}imide, [NTf 2 ] - anion were synthesized and characterized. Their physicochemical properties, such as density, viscosity and ionic conductivity, electrochemical window, along with thermal properties including phase transition behavior and decomposition temperature, have been measured. All of these ILs showed large liquid range temperature, low viscosity, and good conductivity. Additionally, by combining DFT calculations along with electrochemical characterization it appears that these novel ILs show good electrochemical stability windows, suitable for the potential application as electrolyte materials in electrochemical energy storage devices. ©2016 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

One-pot hydrothermal synthesis of zirconium dioxide nanoparticles decorated reduced graphene oxide composite as high performance electrochemical sensing and biosensing platform

International Nuclear Information System (INIS)

Teymourian, Hazhir; Salimi, Abdollah; Firoozi, Somayeh; Korani, Aazam; Soltanian, Saied

2014-01-01

Graphical abstract: - Highlights: • One pot hydrothermal synthesis used for preparing of ZrO 2 NPs reduced graphene oxide. • Electrocatalytic activity of ZrO 2 /rGO improved in compared to ZrO 2 based C- materials. • ZrO 2 NPs/rGO modified GCE was used for electrocatalytic reduction of O 2 and H 2 O 2 . • ZrO 2 NPs/rGO/GCE shows excellent ability to simultaneous detection of AA,UA and DP. • With immobilization of GOX onto ZrO 2 NPs/rGO a sensitive glucose biosensor fabricated. - Abstract: We report on the synthesis of zirconium dioxide-reduced graphene oxide composite (ZrO 2 -rGO) and its application as a novel architecture for electrochemical sensing and biosensing purposes. ZrO 2 -rGO hybrid is synthesized through a simple one-step hydrothermal route, where the reduction of GO and the in-situ generation of ZrO 2 nanoparticles (NPs) occurred simultaneously. Characterization of the resultant hybrid material using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman spectroscopy clearly indicated the homogeneous dispersion of ZrO 2 NPs with particle sizes of ∼5 nm on rGO sheets. The potential application of ZrO 2 -rGO modified glassy carbon electrode (ZrO 2 -rGO/GC) for electroanalytical purposes was demonstrated by using several important electroactive compounds as representative examples (i.e., O 2 , hydrogen peroxide (H 2 O 2 ), glucose, ascorbic acid (AA), dopamine (DA) and uric acid (UA)). Electrochemical control experiments by using different composites of ZrO 2 /graphite, ZrO 2 /Active Carbon and ZrO 2 electrodeposited on activated GC electrode revealed that the ZrO 2 -rGO composite possessed superior electrocatalytic activitiy towards the catalytic reduction of O 2 and H 2 O 2 at more reduced overpotentials. The linear range of H 2 O 2 concentration was from 0.10 to 1340 μM with the detection limit of 20 nM (S/N = 3). Furthermore, via immobilization of glucose oxidase (GOx) enzyme onto the

Synthesis of nitrogen-doped activated graphene aerogel/gold nanoparticles and its application for electrochemical detection of hydroquinone and o-dihydroxybenzene

Science.gov (United States)

Juanjuan, Zhang; Ruiyi, Li; Zaijun, Li; Junkang, Liu; Zhiguo, Gu; Guangli, Wang

2014-04-01

Graphene aerogel materials have attracted increasing attention owing to their large specific surface area, high conductivity and electronic interactions. Here, we report for the first time a novel strategy for the synthesis of nitrogen-doped activated graphene aerogel/gold nanoparticles (N-doped AGA/GNs). First, the mixture of graphite oxide, 2,4,6-trihydroxybenzaldehyde, urea and potassium hydroxide was dispersed in water and subsequently heated to form a graphene oxide hydrogel. Then, the hydrogel was dried by freeze-drying and reduced by thermal annealing in an Ar/H2 environment in sequence. Finally, GNs were adsorbed on the surface of the N-doped AGA. The resulting N-doped AGA/GNs offers excellent electronic conductivity (2.8 × 103 S m-1), specific surface area (1258 m2 g-1), well-defined 3D hierarchical porous structure and apparent heterogeneous electron transfer rate constant (40.78 +/- 0.15 cm s-1), which are notably better than that of previous graphene aerogel materials. Moreover, the N-doped AGA/GNs was used as a new sensing material for the electrochemical detection of hydroquinone (HQ) and o-dihydroxybenzene (DHB). Owing to the greatly enhanced electron transfer and mass transport, the sensor displays ultrasensitive electrochemical response to HQ and DHB. Its differential pulse voltammetric peak current linearly increases with the increase of HQ and DHB in the range of 5.0 × 10-8 to 1.8 × 10-4 M for HQ and 1 × 10-8 to 2.0 × 10-4 M for DHB. The detection limit is 1.5 × 10-8 M for HQ and 3.3 × 10-9 M for DHB (S/N = 3). This method provides the advantage of sensitivity, repeatability and stability compared with other HQ and DHB sensors. The sensor has been successfully applied to detection of HQ and DHB in real water samples with the spiked recovery in the range of 96.8-103.2%. The study also provides a promising approach for the fabrication of various graphene aerogel materials with improved electrochemical performances, which can be potentially

2D nanomaterials based electrochemical biosensors for cancer diagnosis.

Science.gov (United States)

Wang, Lu; Xiong, Qirong; Xiao, Fei; Duan, Hongwei

2017-03-15

Cancer is a leading cause of death in the world. Increasing evidence has demonstrated that early diagnosis holds the key towards effective treatment outcome. Cancer biomarkers are extensively used in oncology for cancer diagnosis and prognosis. Electrochemical sensors play key roles in current laboratory and clinical analysis of diverse chemical and biological targets. Recent development of functional nanomaterials offers new possibilities of improving the performance of electrochemical sensors. In particular, 2D nanomaterials have stimulated intense research due to their unique array of structural and chemical properties. The 2D materials of interest cover broadly across graphene, graphene derivatives (i.e., graphene oxide and reduced graphene oxide), and graphene-like nanomaterials (i.e., 2D layered transition metal dichalcogenides, graphite carbon nitride and boron nitride nanomaterials). In this review, we summarize recent advances in the synthesis of 2D nanomaterials and their applications in electrochemical biosensing of cancer biomarkers (nucleic acids, proteins and some small molecules), and present a personal perspective on the future direction of this area. Copyright © 2016 Elsevier B.V. All rights reserved.

Controlling the properties of graphene produced by electrochemical exfoliation

International Nuclear Information System (INIS)

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

2015-01-01

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

Automated electrochemical assembly of the protected potential TMG-chitotriomycin precursor based on rational optimization of the carbohydrate building block.

Science.gov (United States)

Nokami, Toshiki; Isoda, Yuta; Sasaki, Norihiko; Takaiso, Aki; Hayase, Shuichi; Itoh, Toshiyuki; Hayashi, Ryutaro; Shimizu, Akihiro; Yoshida, Jun-ichi

2015-03-20

The anomeric arylthio group and the hydroxyl-protecting groups of thioglycosides were optimized to construct carbohydrate building blocks for automated electrochemical solution-phase synthesis of oligoglucosamines having 1,4-β-glycosidic linkages. The optimization study included density functional theory calculations, measurements of the oxidation potentials, and the trial synthesis of the chitotriose trisaccharide. The automated synthesis of the protected potential N,N,N-trimethyl-d-glucosaminylchitotriomycin precursor was accomplished by using the optimized building block.

Optical properties of cadmium sulfide nanocrystal film prepared by electrochemical synthesis at liquid-liquid interface

International Nuclear Information System (INIS)

Luan Yemei; An Maozhong; Lu Guoqi

2006-01-01

Dendritic nanocrystalline CdS film was deposited at liquid-liquid interface of surfactants and an electrolyte containing 4 mmol L -1 cadmium chloride (CdCl 2 ) and 16 mmol L -1 thioacetamide (CH 3 CSNH 2 ) with an initial pH value of 5 at 15 deg. C by electrochemical synthesis. The nanofilm was characterized by transmission electron microscopy (TEM), field emission scanning electron microscope (FE-SEM), atomic force microscopy (AFM), ultraviolet visible (UV-vis) absorption spectroscopy and fluorescence spectroscopy. The surface morphology and particle size of the nanofilm were investigated by AFM, SEM and TEM, and the crystalline size was 30-50 nm. The thickness of the nanofilm calculated by optical absorption spectrum was 80 nm. The microstructure and composition of the nanofilm was investigated by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), showing its polycrystalline structure consisting of CdS and Cd. Optical properties of the nanofilm were investigated systematically by UV-vis absorption and fluorescence spectroscopy. A λ onset blue shift compared with bulk CdS was observed in the absorption spectra. Fluorescence spectra of the nanofilm indicated that the CdS nanofilm emitted blue and green light. The nanocomposites film electrode will bring about anodic photocurrent during illumination, showing that the transfer of cavities produces photocurrent

Iron-Based Nanomaterials/Graphene Composites for Advanced Electrochemical Sensors

Directory of Open Access Journals (Sweden)

Kaveh Movlaee

2017-11-01

Full Text Available Iron oxide nanostructures (IONs in combination with graphene or its derivatives—e.g., graphene oxide and reduced graphene oxide—hold great promise toward engineering of efficient nanocomposites for enhancing the performance of advanced devices in many applicative fields. Due to the peculiar electrical and electrocatalytic properties displayed by composite structures in nanoscale dimensions, increasing efforts have been directed in recent years toward tailoring the properties of IONs-graphene based nanocomposites for developing more efficient electrochemical sensors. In the present feature paper, we first reviewed the various routes for synthesizing IONs-graphene nanostructures, highlighting advantages, disadvantages and the key synthesis parameters for each method. Then, a comprehensive discussion is presented in the case of application of IONs-graphene based composites in electrochemical sensors for the determination of various kinds of (biochemical substances.

Iron-Based Nanomaterials/Graphene Composites for Advanced Electrochemical Sensors

Science.gov (United States)

Movlaee, Kaveh; Ganjali, Mohmmad Reza; Norouzi, Parviz

2017-01-01

Iron oxide nanostructures (IONs) in combination with graphene or its derivatives—e.g., graphene oxide and reduced graphene oxide—hold great promise toward engineering of efficient nanocomposites for enhancing the performance of advanced devices in many applicative fields. Due to the peculiar electrical and electrocatalytic properties displayed by composite structures in nanoscale dimensions, increasing efforts have been directed in recent years toward tailoring the properties of IONs-graphene based nanocomposites for developing more efficient electrochemical sensors. In the present feature paper, we first reviewed the various routes for synthesizing IONs-graphene nanostructures, highlighting advantages, disadvantages and the key synthesis parameters for each method. Then, a comprehensive discussion is presented in the case of application of IONs-graphene based composites in electrochemical sensors for the determination of various kinds of (bio)chemical substances. PMID:29168771

An electrochemical approach: Switching Structures of rare earth metal Praseodymium hexacyanoferrate and its application to sulfite sensor in Red Wine

International Nuclear Information System (INIS)

Devadas, Balamurugan; Sivakumar, Mani; Chen, Shen Ming; Cheemalapati, Srikanth

2015-01-01

Graphical abstract: Nucleation and growth of PrHCF and its application to sulfite oxidation in wine samples. - Highlights: • Electrochemical synthesis of PrHCF. • Switching structures of PrHCF. • Sulfite electrochemical sensor. • Wide linear range and low limit of detection. • Real sample application. - Abstract: Herein, we report a shape-controlled preparation of Praseodymium hexacyanoferrate (PrHCF) using a simple electrochemical technique. The electrochemically fabricated PrHCF modified glassy carbon electrodes (GCE) shows an excellent electrocatalytic activity towards sulfite oxidation. The morphology of PrHCF particles were controlled by carefully changing various synthesis conditions including electrochemical technique (cyclic voltammetry, amperometry and chemical), cations in the supporting electrolyte (K + , Na + , Li + and H + ), deposition cycles, molar ratio of precursors, and applied potential (-.2,0 and 0.2 V). The morphologies of the PrHCF was elucidated using scanning electron microscopy (SEM). The as-synthesized PrHCF was characterized using X-ray diffraction pattern (XRD), Infra-red (IR) and energy dispersive X-ray spectroscopy (EDX). The electrochemical oxidation of sulfite on PrHCF modified GCE was investigated using cyclic voltammetry (CV) and linear sweep voltammetry (LSV). The sensitivity of the as-developed sulfite sensor was determined to be 0.036 μA μM −1 cm −2 . The low limit of detection was determined to be 2.15 μM. The real time application of PrHCF modified GCE was confirmed through the determination of sulfite from red wine and tap water samples

Electrochemical and spectroscopic studies of tungstencarbonyl complexes containing nitrogen and phosphorous ligands

Directory of Open Access Journals (Sweden)

Haddad Paula S.

2000-01-01

Full Text Available The present work deals with the synthesis, spectroscopic investigation and electrochemical behaviour of the compounds [W(CO4(bipy] (1, [W(CO3(bipy(dppm] (2 and [W(CO3(bipy(dppf] (3, bipy = 2,2'-bipyridine; dppm = bis(diphenylphosphinomethane; dppf = 1,1'-bis(diphenylphosphinoferrocene. The IR and 31P{¹H} NMR spectroscopic data have shown an octahedral coordination geometry for the tungsten atom with the diphosphines acting as monodentate ligands. The electrochemical behaviour of the complexes was investigated by cyclic voltammetry and controlled potential coulometry. Cyclic voltammograms have indicated that the compounds containing diphosphines ligands are more stable towards oxidation than compound (1.

Electrochemical supercapacitors from conducting polyaniline-graphene platforms.

Science.gov (United States)

Ashok Kumar, Nanjundan; Baek, Jong-Beom

2014-06-18

Energy storage devices such as electrochemical supercapacitors, with high power and energy densities are required to address the colossal energy requirements against the backdrop of global warming and the looming energy crisis. Nanocarbon, particularly two-dimensional graphene and graphene-based conducting polymer composites are promising electrode materials for such energy storage devices. Owing to their environmental stability, the low cost of polymers with high electroactivity and pseudocapacitance, such composite hybrids are expected to have wide implications in next generation clean and efficient energy systems. In this feature article, an overview of current research and important advances over the past four years on the development of conducting polyaniline (PANI)-graphene based composite electrodes for electrochemical supercapacitors are highlighted. Particular emphasis is made on the design, fabrication and assembly of nanostructured electrode architectures comprising PANI and graphene along with metal oxides/hydroxides and carbon nanotubes. Comments on the challenges and perspectives towards rational design and synthesis of graphene-based conducting polymer composites for energy storage are discussed.

Controllable synthesis of hierarchical nickel cobalt sulfide with enhanced electrochemical activity

Science.gov (United States)

Tie, Jinjin; Han, Jiaxi; Diao, Guiqiang; Liu, Jiwen; Xie, Zhuopeng; Cheng, Gao; Sun, Ming; Yu, Lin

2018-03-01

The composition of nickel cobalt sulfide has great influence on its electrochemical performance. Herein, the nickel cobalt sulfide with different composition and mixed phase were synthesized by one-step solvothermal method through changing the molar ratio of Ni to Co in the reaction system. The electrochemical measurements showed that the nickel cobalt sulfide with a theoretical molar ratio of Ni/Co to be 1.5:1.5 (NCS-2) demonstrates the superior pseudocapacitive performance with a high specific capacitance (6.47 F cm-2 at 10 mA cm-2) and a favorable Coulombic efficiency (∼99%). Whereas, when applied as the catalyst for hydrogen evolution reaction in 1 M KOH aqueous electrolyte, the nickel cobalt sulfide with a theoretical molar ratio of Ni/Co is 1:2 (NCS-1) displays better catalytic activity, and it requires a relatively lower overpotential of 282 mV to deliver the current density of 10 mA cm-2.

EDTA assisted synthesis of hydroxyapatite nanoparticles for electrochemical sensing of uric acid

International Nuclear Information System (INIS)

Kanchana, P.; Sekar, C.

2014-01-01

Hydroxyapatite nanoparticles have been synthesized using EDTA as organic modifier by a simple microwave irradiation method and its application for the selective determination of uric acid (UA) has been demonstrated. Electrochemical behavior of uric acid at HA nanoparticle modified glassy carbon electrode (E-HA/GCE) has been investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), linear sweep voltammetry (LSV) and amperometry. The E-HA modified electrode exhibits efficient electrochemical activity towards uric acid sensing without requiring enzyme or electron mediator. Amperometry studies revealed that the fabricated electrode has excellent sensitivity for uric acid with the lowest detection limit of 142 nM over a wide concentration range from 1 × 10 −7 to 3 × 10 −5 M. Moreover, the studied E-HA modified GC electrode exhibits a good reproducibility and long-term stability and an admirable selectivity towards the determination of UA even in the presence of potential interferents. The analytical performance of this sensor was evaluated for the detection of uric acid in human urine and blood serum samples. - Highlights: • EDTA- hydroxyapatite (HA) nanoparticles have been synthesized by microwave irradiation method. • A novel amperometric Uric Acid biosensor has been fabricated using E-HA/GCE. • The fabricated sensor exhibits a wide linear range, good stability and high reproducibility. • The sensor was applied for the detection of UA in human blood serum and urine

Nitrogen-doped reduced graphene oxide electrodes for electrochemical supercapacitors.

Science.gov (United States)

Nolan, Hugo; Mendoza-Sanchez, Beatriz; Ashok Kumar, Nanjundan; McEvoy, Niall; O'Brien, Sean; Nicolosi, Valeria; Duesberg, Georg S

2014-02-14

Herein we use Nitrogen-doped reduced Graphene Oxide (N-rGO) as the active material in supercapacitor electrodes. Building on a previous work detailing the synthesis of this material, electrodes were fabricated via spray-deposition of aqueous dispersions and the electrochemical charge storage mechanism was investigated. Results indicate that the functionalised graphene displays improved performance compared to non-functionalised graphene. The simplicity of fabrication suggests ease of up-scaling of such electrodes for commercial applications.

A new electrochemically responsive 2D π-conjugated covalent organic framework as a high performance supercapacitor

KAUST Repository

Das, Sabuj Kanti

2018-03-02

Covalent organic frameworks (COFs) build via periodic arrangement of organic building blocks are attracting increasing interest in recent times due to the huge scope in their synthesis through a wide range of structural motifs and diversity in their potential applications. Here we report the synthesis of a new porous extended network π-conjugated TFP-NDA-COF via solvothermal Schiff base condensation of 1,3,5-triformylphloroglucinol (TFP) with 1,5-diaminonaphthalene (NDA). The electrochemical study demonstrates that TFP-NDA-COF has the capability of energy storage up to 379 F g−1 at 2 mV s−1 scan rate, 348 F g−1 at 0.5 A g−1 and offer excellent specific capacitance retention of 75% after 8000 charge discharge cycles. High electrochemical performance could be attributed to the π-electronic conjugation along the polymeric 2D layered network and ion conduction inside the porous channel and permanent porosity of the framework. This indicates that the COF reported herein meets the key requirements like energy storage ability and electrochemical stability needed for developing an efficient energy storage device.

A new electrochemically responsive 2D π-conjugated covalent organic framework as a high performance supercapacitor

KAUST Repository

Das, Sabuj Kanti; Bhunia, Kousik; Mallick, Arijit; Pradhan, Anirban; Pradhan, Debabrata; Bhaumik, Asim

2018-01-01

Covalent organic frameworks (COFs) build via periodic arrangement of organic building blocks are attracting increasing interest in recent times due to the huge scope in their synthesis through a wide range of structural motifs and diversity in their potential applications. Here we report the synthesis of a new porous extended network π-conjugated TFP-NDA-COF via solvothermal Schiff base condensation of 1,3,5-triformylphloroglucinol (TFP) with 1,5-diaminonaphthalene (NDA). The electrochemical study demonstrates that TFP-NDA-COF has the capability of energy storage up to 379 F g−1 at 2 mV s−1 scan rate, 348 F g−1 at 0.5 A g−1 and offer excellent specific capacitance retention of 75% after 8000 charge discharge cycles. High electrochemical performance could be attributed to the π-electronic conjugation along the polymeric 2D layered network and ion conduction inside the porous channel and permanent porosity of the framework. This indicates that the COF reported herein meets the key requirements like energy storage ability and electrochemical stability needed for developing an efficient energy storage device.

Solid oxide electrochemical reactor science.

Energy Technology Data Exchange (ETDEWEB)

Sullivan, Neal P. (Colorado School of Mines, Golden, CO); Stechel, Ellen Beth; Moyer, Connor J. (Colorado School of Mines, Golden, CO); Ambrosini, Andrea; Key, Robert J. (Colorado School of Mines, Golden, CO)

2010-09-01

Solid-oxide electrochemical cells are an exciting new technology. Development of solid-oxide cells (SOCs) has advanced considerable in recent years and continues to progress rapidly. This thesis studies several aspects of SOCs and contributes useful information to their continued development. This LDRD involved a collaboration between Sandia and the Colorado School of Mines (CSM) ins solid-oxide electrochemical reactors targeted at solid oxide electrolyzer cells (SOEC), which are the reverse of solid-oxide fuel cells (SOFC). SOECs complement Sandia's efforts in thermochemical production of alternative fuels. An SOEC technology would co-electrolyze carbon dioxide (CO{sub 2}) with steam at temperatures around 800 C to form synthesis gas (H{sub 2} and CO), which forms the building blocks for a petrochemical substitutes that can be used to power vehicles or in distributed energy platforms. The effort described here concentrates on research concerning catalytic chemistry, charge-transfer chemistry, and optimal cell-architecture. technical scope included computational modeling, materials development, and experimental evaluation. The project engaged the Colorado Fuel Cell Center at CSM through the support of a graduate student (Connor Moyer) at CSM and his advisors (Profs. Robert Kee and Neal Sullivan) in collaboration with Sandia.

Electrochemical synthesis of novel polymer based on (4-(2,3-dihydrothieno[3,4-6][1,4][dioxin-5-yl) aniline) in aqueous solution: Characterization and application

Energy Technology Data Exchange (ETDEWEB)

Shahhosseini, Leyla [Chemistry Department, Kerman Branch, Islamic Azad University, Kerman (Iran, Islamic Republic of); Nateghi, Mohammad Reza, E-mail: mnateghi@iauyazd.ac.ir [Chemistry Department, Yazd Branch, Islamic Azad University, Yazd (Iran, Islamic Republic of); Kazemipour, Maryam [Chemistry Department, Kerman Branch, Islamic Azad University, Kerman (Iran, Islamic Republic of); Borhani Zarandi, Mahmoud [Department of Physics, Yazd University, P.O. Box 97175/615, Yazd (Iran, Islamic Republic of)

2016-07-01

4-(2,3-dihydrothieno[3,4-6][1,4][dioxin-5-yl) aniline, an interesting novel monomer was successfully synthesized in which α-carbon on ethylenedioxythiophene was linked to aniline at para position. The structure of the monomer was approved by infrared (IR), gas chromatography-mass spectrometry (GC-MS) and {sup 1}H nuclear magnetic resonance ({sup 1}H NMR) spectroscopies. Poly (4-(2,3-dihydrothieno[3,4-6][1,4][dioxin-5-yl) aniline) and its composite with graphene were electrochemically synthesized in aqueous solution by cyclic potential sweep method. The Polymer was characterized by IR and UV–vis spectroscopies, scanning electron microscopy, cyclic voltammetry, and electrochemical impedance spectroscopy techniques. Electrochemical synthesis conditions were optimized to prepare high conducting and porous polymer so it can be efficiently used as a counter electrode in fabrication of dye sensitized solar cells. Photovoltaic experiments revealed that energy conversion efficiency of the solar cell fabricated using polymer composite (7.52%) is 21% greater than that prepared by Pt counter electrode (6.19%). - Highlights: • A Novel monomer comprising aniline and EDOT was synthesized by a simple process. • Poly (ANI-EDOT) was synthesized and characterized by cyclic potential sweep method. • The copolymer changes from yellow at −0.9 V to dark green color at +0.9 V reversibly. • Poly (ANI-EDOT)/graphene is porous with electrocatalytic effect on I{sub 3}{sup −} reduction.

Electrochemical synthesis of novel polymer based on (4-(2,3-dihydrothieno[3,4-6][1,4][dioxin-5-yl) aniline) in aqueous solution: Characterization and application

International Nuclear Information System (INIS)

Shahhosseini, Leyla; Nateghi, Mohammad Reza; Kazemipour, Maryam; Borhani Zarandi, Mahmoud

2016-01-01

4-(2,3-dihydrothieno[3,4-6][1,4][dioxin-5-yl) aniline, an interesting novel monomer was successfully synthesized in which α-carbon on ethylenedioxythiophene was linked to aniline at para position. The structure of the monomer was approved by infrared (IR), gas chromatography-mass spectrometry (GC-MS) and "1H nuclear magnetic resonance ("1H NMR) spectroscopies. Poly (4-(2,3-dihydrothieno[3,4-6][1,4][dioxin-5-yl) aniline) and its composite with graphene were electrochemically synthesized in aqueous solution by cyclic potential sweep method. The Polymer was characterized by IR and UV–vis spectroscopies, scanning electron microscopy, cyclic voltammetry, and electrochemical impedance spectroscopy techniques. Electrochemical synthesis conditions were optimized to prepare high conducting and porous polymer so it can be efficiently used as a counter electrode in fabrication of dye sensitized solar cells. Photovoltaic experiments revealed that energy conversion efficiency of the solar cell fabricated using polymer composite (7.52%) is 21% greater than that prepared by Pt counter electrode (6.19%). - Highlights: • A Novel monomer comprising aniline and EDOT was synthesized by a simple process. • Poly (ANI-EDOT) was synthesized and characterized by cyclic potential sweep method. • The copolymer changes from yellow at −0.9 V to dark green color at +0.9 V reversibly. • Poly (ANI-EDOT)/graphene is porous with electrocatalytic effect on I_3"− reduction.

Production of bioelectricity, bio-hydrogen, high value chemicals and bioinspired nanomaterials by electrochemically active biofilms.

Science.gov (United States)

Kalathil, Shafeer; Khan, Mohammad Mansoob; Lee, Jintae; Cho, Moo Hwan

2013-11-01

Microorganisms naturally form biofilms on solid surfaces for their mutual benefits including protection from environmental stresses caused by contaminants, nutritional depletion or imbalances. The biofilms are normally dangerous to human health due to their inherited robustness. On the other hand, a recent study suggested that electrochemically active biofilms (EABs) generated by electrically active microorganisms have properties that can be used to catalyze or control the electrochemical reactions in a range of fields, such as bioenergy production, bioremediation, chemical/biological synthesis, bio-corrosion mitigation and biosensor development. EABs have attracted considerable attraction in bioelectrochemical systems (BESs), such as microbial fuel cells and microbial electrolysis cells, where they act as living bioanode or biocathode catalysts. Recently, it was reported that EABs can be used to synthesize metal nanoparticles and metal nanocomposites. The EAB-mediated synthesis of metal and metal-semiconductor nanocomposites is expected to provide a new avenue for the greener synthesis of nanomaterials with high efficiency and speed than other synthetic methods. This review covers the general introduction of EABs, as well as the applications of EABs in BESs, and the production of bio-hydrogen, high value chemicals and bio-inspired nanomaterials. Copyright © 2013 Elsevier Inc. All rights reserved.

Obtention of superconductivity by room temperature electrochemical oxidation of La2CuO4

International Nuclear Information System (INIS)

Casan-Pastor, N.; Fuertes, A.; Gomez-Romero, P.

1993-01-01

The undoped oxide La2CuO4 has required traditionally synthesis under high pressure of oxygen (and high temperatures) to incorporate excess oxygen into its structure and become a superconductor. The electrochemical oxidation of this same oxide at room temperature and pressure constitutes a striking example of the use of an alternative driving force for the oxidation of oxides to become superconductors. Electrochemical treatment of oxides has been frequently applied to their reduction with cationic intercalation. Oxidations of these solid with the concomitant intercalation of anions into their lattice shows also great promises. The paper reports recent results in the electrochemical oxidation of La2CuO4 and other cuprates, showing also the important role of post-oxidation thermal treatments on the properties of the resulting solids

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

International Nuclear Information System (INIS)

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

2013-01-01

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

Estrone specific molecularly imprinted polymeric nanospheres: synthesis, characterization and applications for electrochemical sensor development.

Science.gov (United States)

Congur, Gulsah; Senay, Hilal; Turkcan, Ceren; Canavar, Ece; Erdem, Arzum; Akgol, Sinan

2013-06-28

The aim of this study is (i) to prepare estrone-imprinted nanospheres (nano-EST-MIPs) and (ii) to integrate them into the electrochemical sensor as a recognition layer. N-methacryloyl-(l)-phenylalanine (MAPA) was chosen as the complexing monomer. Firstly, estrone (EST) was complexed with MAPA and the EST-imprinted poly(2-hyroxyethylmethacrylate-co-N-methacryloyl-(l)-phenylalanine) [EST-imprinted poly(HEMA-MAPA)] nanospheres were synthesized by surfactant- free emulsion polymerization method. The specific surface area of the EST-imprinted poly(HEMA-MAPA) nanospheres was found to be 1275 m2/g with a size of 163.2 nm in diameter. According to the elemental analysis results, the nanospheres contained 95.3 mmole MAPA/g nanosphere. The application of EST specific MIP nanospheres for the development of an electrochemical biosensor was introduced for the first time in our study by using electrochemical impedance spectroscopy (EIS) technique. This nano-MIP based sensor presented a great specificity and selectivity for EST.

Electrochemical Synthesis of Mesoporous CoPt Nanowires for Methanol Oxidation

Directory of Open Access Journals (Sweden)

Albert Serrà

2014-03-01

Full Text Available A new electrochemical method to synthesize mesoporous nanowires of alloys has been developed. Electrochemical deposition in ionic liquid-in-water (IL/W microemulsion has been successful to grow mesoporous CoPt nanowires in the interior of polycarbonate membranes. The viscosity of the medium was high, but it did not avoid the entrance of the microemulsion in the interior of the membrane’s channels. The structure of the IL/W microemulsions, with droplets of ionic liquid (4 nm average diameter dispersed in CoPt aqueous solution, defined the structure of the nanowires, with pores of a few nanometers, because CoPt alloy deposited only from the aqueous component of the microemulsion. The electrodeposition in IL/W microemulsion allows obtaining mesoporous structures in which the small pores must correspond to the size of the droplets of the electrolytic aqueous component of the microemulsion. The IL main phase is like a template for the confined electrodeposition. The comparison of the electrocatalytic behaviours towards methanol oxidation of mesoporous and compact CoPt nanowires of the same composition, demonstrated the porosity of the material. For the same material mass, the CoPt mesoporous nanowires present a surface area 16 times greater than compact ones, and comparable to that observed for commercial carbon-supported platinum nanoparticles.

EDTA assisted synthesis of hydroxyapatite nanoparticles for electrochemical sensing of uric acid

Energy Technology Data Exchange (ETDEWEB)

Kanchana, P.; Sekar, C., E-mail: Sekar2025@gmail.com

2014-09-01

Hydroxyapatite nanoparticles have been synthesized using EDTA as organic modifier by a simple microwave irradiation method and its application for the selective determination of uric acid (UA) has been demonstrated. Electrochemical behavior of uric acid at HA nanoparticle modified glassy carbon electrode (E-HA/GCE) has been investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), linear sweep voltammetry (LSV) and amperometry. The E-HA modified electrode exhibits efficient electrochemical activity towards uric acid sensing without requiring enzyme or electron mediator. Amperometry studies revealed that the fabricated electrode has excellent sensitivity for uric acid with the lowest detection limit of 142 nM over a wide concentration range from 1 × 10{sup −7} to 3 × 10{sup −5} M. Moreover, the studied E-HA modified GC electrode exhibits a good reproducibility and long-term stability and an admirable selectivity towards the determination of UA even in the presence of potential interferents. The analytical performance of this sensor was evaluated for the detection of uric acid in human urine and blood serum samples. - Highlights: • EDTA- hydroxyapatite (HA) nanoparticles have been synthesized by microwave irradiation method. • A novel amperometric Uric Acid biosensor has been fabricated using E-HA/GCE. • The fabricated sensor exhibits a wide linear range, good stability and high reproducibility. • The sensor was applied for the detection of UA in human blood serum and urine.

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

International Nuclear Information System (INIS)

Wen, Yong; Pei, Lizhai; Wei, Tian

2017-01-01

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

Fungal nanoscale metal carbonates and production of electrochemical materials.

Science.gov (United States)

Li, Qianwei; Gadd, Geoffrey Michael

2017-09-01

Fungal biomineralization of carbonates results in metal removal from solution or immobilization within a solid matrix. Such a system provides a promising method for removal of toxic or valuable metals from solution, such as Co, Ni, and La, with some carbonates being of nanoscale dimensions. A fungal Mn carbonate biomineralization process can be applied for the synthesis of novel electrochemical materials. © 2017 The Authors. Microbial Biotechnology published by John Wiley & Sons Ltd and Society for Applied Microbiology.

Graphene–Gold Nanoparticles Hybrid—Synthesis, Functionalization, and Application in a Electrochemical and Surface-Enhanced Raman Scattering Biosensor

Directory of Open Access Journals (Sweden)

Ibrahim Khalil

2016-05-01

Full Text Available Graphene is a single-atom-thick two-dimensional carbon nanosheet with outstanding chemical, electrical, material, optical, and physical properties due to its large surface area, high electron mobility, thermal conductivity, and stability. These extraordinary features of graphene make it a key component for different applications in the biosensing and imaging arena. However, the use of graphene alone is correlated with certain limitations, such as irreversible self-agglomerations, less colloidal stability, poor reliability/repeatability, and non-specificity. The addition of gold nanostructures (AuNS with graphene produces the graphene–AuNS hybrid nanocomposite which minimizes the limitations as well as providing additional synergistic properties, that is, higher effective surface area, catalytic activity, electrical conductivity, water solubility, and biocompatibility. This review focuses on the fundamental features of graphene, the multidimensional synthesis, and multipurpose applications of graphene–Au nanocomposites. The paper highlights the graphene–gold nanoparticle (AuNP as the platform substrate for the fabrication of electrochemical and surface-enhanced Raman scattering (SERS-based biosensors in diverse applications as well as SERS-directed bio-imaging, which is considered as an emerging sector for monitoring stem cell differentiation, and detection and treatment of cancer.

Electrochemical synthesis of highly crystalline copper nanowires

International Nuclear Information System (INIS)

Kaur, Amandeep; Gupta, Tanish; Kumar, Akshay; Kumar, Sanjeev; Singh, Karamjeet; Thakur, Anup

2015-01-01

Copper nanowires were fabricated within the pores of anodic alumina template (AAT) by template synthesis method at pH = 2.9. X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used to investigate the structure, morphology and composition of fabricated nanowires. These characterizations revealed that the deposited copper nanowires were highly crystalline in nature, dense and uniform. The crystalline copper nanowires are promising in application of future nanoelectronic devices and circuits

Synthesis and electrochemical characterization of stabilized nickel nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Dominguez-Crespo, M.A.; Ramirez-Meneses, E.; Torres Huerta, A.M. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, CICATA-IPN Unidad Altamira, Carretera Tampico-Puerto Industrial, C.P. 89600 Altamira, Tamaulipas (Mexico); Montiel-Palma, V. [Centro de Investigaciones Quimicas, Universidad Autonoma del Estado de Morelos, Av. Universidad 1001, Colonia Chamilpa, C.P.62201 Cuernavaca, Morelos (Mexico); Dorantes Rosales, H. [Departamento de Metalurgia, Escuela Superior de Ingenieria Quimica e Industrias Extractivas - IPN, C.P. 07300, D.F. (Mexico)

2009-02-15

Nickel stabilized nanoparticles produced by an organometallic approach (Chaudret's method) starting from the complex Ni(1,5-COD){sub 2} were used as electrode materials for hydrogen evolution in NaOH at two temperatures (298 and 323 K). The synthesis of the nickel nanoparticles was performed in the presence of two different stabilizers, 1,3-diaminopropane (DAP) and anthranilic acid (AA), by varying the molar ratios (1:1, 1:2 and 1:5 metal:ligand) in order to evaluate their influence on the shape, dispersion, size and electrocatalytic activity of the metallic particles. The presence of an appropriate amount of stabilizer is an effective alternative to the synthesis of small monodispersed metal nanoparticles with diameters around 5 and 8 nm for DAP and AA, respectively. The results are discussed in terms of morphology and the surface state of the nanoparticles. The importance of developing a well-controlled synthetic method which results in higher performances of the resulting nanoparticles is highlighted. Herein we found that the performance with respect to the HER of the Ni electrodes dispersed on a carbon black Vulcan substrate is active and comparable to that reported in the literature for the state-of-the-art electrocatalysts. Appreciable cathodic current densities of {proportional_to}240 mA cm{sup -2} were measured with highly dispersed nickel particles (Ni-5{sub DAP}). This work demonstrates that the aforementioned method can be extended to the preparation of highly active stabilized metal particles without inhibiting the electron transfer for the HER reaction, and it could also be applied to the synthesis of bimetallic nanoparticles. (author)

Facile Synthesis of Boron-doped Graphene Nanosheets with Hierarchical Microstructure at Atmosphere Pressure for Metal-free Electrochemical Detection of Hydrogen Peroxide

International Nuclear Information System (INIS)

Yeh, Min-Hsin; Li, Yan-Sheng; Chen, Guan-Lin; Lin, Lu-Yin; Li, Ta-Jen; Chuang, Hui-Min; Hsieh, Cheng-Yu; Lo, Shen-Chuan; Chiang, Wei-Hung; Ho, Kuo-Chuan

2015-01-01

Graphical abstract: Display Omitted -- Highlights: • B-doped graphene nanosheets (BGNs) were used as a catalyst for sensing H 2 O 2 . • BGNs were synthesized by an atmospheric-pressure carbothermal reaction. • BGNs with hierarchical microstructure provide more electron transport pathways. • B atoms act as the active sites by transferring charges to neighboring C atoms. • Electrocatalytic ability of BGNs was characterized by a rotating disk electrode. -- Abstract: Hydrogen peroxide (H 2 O 2 ) is an essential mediator for most of the oxidative biological reactions in enzyme-based biosensor systems, such as glucose oxidase, cholesterol oxidase, and alcohol oxidase. Synthesis of new catalysts to detect the concentration of H 2 O 2 more precisely is indispensable for enzyme-based electrochemical biosensors. In this study, boron-doped graphene nanosheets (BGNs) with 2.2 atomic percentage (at%) boron doping level and a hierarchical microstructure were synthesized by an atmospheric-pressure carbothermal reaction as a noble-metal free catalyst for sensing H 2 O 2 . The isolated boron atoms on the BGNs surface act as the electrocatalytic sites by transferring charges to neighbor carbon atoms, and the hierarchical microstructure provides multidimensional electron transport pathways for charge transfer and therefore enhances the electrocatalytic ability. BGNs possess a higher reduction current in the cyclic voltammetry (CV) measurement than that of pristine graphene nanosheets (GNs) over the detection range of 0.0 to 10.0 mM at −0.4 V (vs. Ag/AgCl). The BGNs modified electrochemical sensor shows a linear range from 1.0 to 20.0 mM of H 2 O 2 with a sensitivity of 266.7 ± 3.8 μA mM −1 cm −2 and limit of detection (LOD) of 3.8 μM at a signal-to-noise (S/N) ratio of 3. The beneficial hierarchical microstructure and the synergetic effects arising from doping boron in GNs accomplish the better performance of the BGNs modified electrochemical sensor

Electrochemical deposition of thin nano-structured layers of CuInS2 for photovoltaic cells

International Nuclear Information System (INIS)

Cayzac, R.; Boulc'h, F.; Knauth, P.

2006-01-01

In this work, it has been shown that the electrochemical deposition seems to be a promising synthesis technique because the thickness of the layers and their morphology are well adapted to the photovoltaic application. The example of CuInS 2 has been taken. (O.M.)

Use of organic precursors and graphenes in the controlled synthesis of carbon-containing nanomaterials for energy storage and conversion.

Science.gov (United States)

Yang, Shubin; Bachman, Robert E; Feng, Xinliang; Müllen, Klaus

2013-01-15

The development of high-performance electrochemical energy storage and conversion devices, including supercapacitors, lithium-ion batteries, and fuel cells, is an important step on the road to alternative energy technologies. Carbon-containing nanomaterials (CCNMs), defined here as pure carbon materials and carbon/metal (oxide, hydroxide) hybrids with structural features on the nanometer scale, show potential application in such devices. Because of their pronounced electrochemical activity, high chemical and thermal stability and low cost, researchers are interested in CCNMs to serve as electrodes in energy-related devices. Various all-carbon materials are candidates for electrochemical energy storage and conversion devices. Furthermore, carbon-based hybrid materials, which consist of a carbon component with metal oxide- or metal hydroxide-based nanostructures, offer the opportunity to combine the attractive properties of these two components and tune the behavior of the resulting materials. As such, the design and synthesis of CCNMs provide an attractive route for the construction of high-performance electrode materials. Studies in these areas have revealed that both the composition and the fabrication protocol employed in preparing CCNMs influence the morphology and microstructure of the resulting material and its electrochemical performance. Consequently, researchers have developed several synthesis strategies, including hard-templated, soft-templated, and template-free synthesis of CCNMs. In this Account, we focus on recent advances in the controlled synthesis of such CCNMs and the potential of the resulting materials for energy storage or conversion applications. The Account is divided into four major categories based on the carbon precursor employed in the synthesis: low molecular weight organic or organometallic molecules, hyperbranched or cross-linked polymers consisting of aromatic subunits, self-assembling discotic molecules, and graphenes. In each case

Synthesis of water dispersible polyaniline/poly(styrenesulfonic acid) modified graphene composite and its electrochemical properties

International Nuclear Information System (INIS)

Luo, Jing; Jiang, Sisi; Liu, Ren; Zhang, Yongjie; Liu, Xiaoya

2013-01-01

A novel water-dispersible polyaniline (PANI)/graphene composite was prepared by the in situ polymerization of aniline on the surface of poly(styrenesulfonic acid) (PSS) coated graphene nanosheets (PSS-GR). The characterization of atomic force microscopy (AFM), transmission electron microscopy (TEM), Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy confirmed the successful synthesis of PANI/PSS-GR composites and strong interaction between PANI and PSS-GR. The as-synthesized PANI/PSS-GR composite is readily dispersible in water and forms a homogeneous aqueous dispersion which is stable for more than one month. More interestingly, PSS-GR can dope PANI effectively and shift its electroactivity to a neutral or even alkaline environment, making them promising candidates for biological application. In addition, the PANI/PSS-GR composite shows improved electrical conductivity and electrochemical stability compared to the neat polyaniline. Furthermore, the potential use of this composite for detection of ascorbic acid (AA) was investigated. A low detection limit of 5 × 10 −6 M and a linear detection range between 1 × 10 −4 M and 1 × 10 −3 M was attained, indicating the high electrocatalytic ability of this composite. Anticipatedly, the synthesized composite will find promising applications as a novel electrode material in sensors and other devices in virtue of their outstanding characteristics of water-dispersibility, good cycle stability, electroactivity in neutral solution and excellent electrocatalytic ability

Porous One-Dimensional Nanomaterials: Design, Fabrication and Applications in Electrochemical Energy Storage.

Science.gov (United States)

Wei, Qiulong; Xiong, Fangyu; Tan, Shuangshuang; Huang, Lei; Lan, Esther H; Dunn, Bruce; Mai, Liqiang

2017-05-01

Electrochemical energy storage technology is of critical importance for portable electronics, transportation and large-scale energy storage systems. There is a growing demand for energy storage devices with high energy and high power densities, long-term stability, safety and low cost. To achieve these requirements, novel design structures and high performance electrode materials are needed. Porous 1D nanomaterials which combine the advantages of 1D nanoarchitectures and porous structures have had a significant impact in the field of electrochemical energy storage. This review presents an overview of porous 1D nanostructure research, from the synthesis by bottom-up and top-down approaches with rational and controllable structures, to several important electrochemical energy storage applications including lithium-ion batteries, sodium-ion batteries, lithium-sulfur batteries, lithium-oxygen batteries and supercapacitors. Highlights of porous 1D nanostructures are described throughout the review and directions for future research in the field are discussed at the end. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Highly stable copper oxide composite as an effective photocathode for water splitting via a facile electrochemical synthesis strategy

KAUST Repository

Zhang, Zhonghai

2012-01-01

. Thus, the electrochemical strategy proposed in this study for the synthesis of the Cu 2O/CuO composite opens a new way to use copper oxides as photocathode materials in PEC cells for a highly stable and effective water splitting. © 2012 The Royal Society of Chemistry.

Advanced Proton Conducting Polymer Electrolytes for Electrochemical Capacitors

Science.gov (United States)

Gao, Han

Research on solid electrochemical energy storage devices aims to provide high performance, low cost, and safe operation solutions for emerging applications from flexible consumer electronics to microelectronics. Polymer electrolytes, minimizing device sealing and liquid electrolyte leakage, are key enablers for these next-generation technologies. In this thesis, a novel proton-conducing polymer electrolyte system has been developed using heteropolyacids (HPAs) and polyvinyl alcohol for electrochemical capacitors. A thorough understanding of proton conduction mechanisms of HPAs together with the interactions among HPAs, additives, and polymer framework has been developed. Structure and chemical bonding of the electrolytes have been studied extensively to identify and elucidate key attributes affecting the electrolyte properties. Numerical models describing the proton conduction mechanism have been applied to differentiate those attributes. The performance optimization of the polymer electrolytes through additives, polymer structural modifications, and synthesis of alternative HPAs has achieved several important milestones, including: (a) high proton mobility and proton density; (b) good ion accessibility at electrode/electrolyte interface; (c) wide electrochemical stability window; and (d) good environmental stability. Specifically, high proton mobility has been addressed by cross-linking the polymer framework to improve the water storage capability at normal-to-high humidity conditions (e.g. 50-80% RH) as well as by incorporating nano-fillers to enhance the water retention at normal humidity levels (e.g. 30-60% RH). High proton density has been reached by utilizing additional proton donors (i.e. acidic plasticizers) and by developing different HPAs. Good ion accessibility has been achieved through addition of plasticizers. Electrochemical stability window of the electrolyte system has also been investigated and expanded by utilizing HPAs with different heteroatoms

Microwave synthesis of metal nanocatalysts for the electrochemical oxidation of small biomolecules

DEFF Research Database (Denmark)

Jensen, Kathrine Schiørring Steen; Sun, Hongyu; Werchmeister, Rebecka Maria Larsen

2017-01-01

Electrochemical oxidation of small biomolecules provides an approach to generate clean energy from a sustainable resource. It serves as a principle for anode reactions in fuel cells to convert energy stored in chemical bonds into electrical power. Efficient and robust nanocatalysts are essential ...

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-07-15

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

A fast chemical route for the synthesis of TBHQ functionalized reduced graphene oxide and its electrochemical performances

Energy Technology Data Exchange (ETDEWEB)

Rana, Subhasis; Sen, Pintu, E-mail: psen@vecc.gov.in; Bandyopadhyay, S.K.

2016-02-01

A fast chemical route for the synthesis of tertiary butyl hydroquinone (TBHQ) functionalized reduced graphene oxide (FRGO) and their application as high performance electrode materials for supercapacitors have been reported. Reductions of chemically exfoliated graphene oxides (GO) in the presence of small amount of TBHQ (1–2 wt % with respect to GO) at various time periods were investigated through XRD, FTIR and Raman studies. Reappearance of broad diffraction peak close to graphite peak (002) reveals an efficient method of reduction of different oxygen containing functional groups present in GO/FGO resulting in a decrease of interlayer d-spacing (∼3.5 Å). Absence of the absorption peaks in FTIR for –C=O, t-O–H, epoxide and alkoxy groups supports the complete reduction of GO to FRGO by hydrazine hydrate within a short time period of 4 h reduction under reflux condition. A large red shift in UV spectrum of FRGO – 4 h (270 nm) reveals the complete reduction of graphene oxide. The average crystallite sp{sup 2} domains sizes have been estimated through Raman spectroscopy. Plausible mechanism of TBHQ assisted fast chemical reduction of FGO has been enumerated. 1.5 wt % TBHQ in FRGO shows the best electrochemical performance where TBHQ not only acts as a reducing agent during functionalization, but also plays as an active redox molecule for enhanced capacitance of 200 F/g. - Highlights: • A fast chemical route has been adopted for the synthesis of TBHQ functionalized RGO. • The kinetics of chemical reduction becomes faster in the presence of TBHQ. • The FTIR spectrum of functionalized RGO supports the complete reduction process. • TBHQ also plays a vital role for enhancing capacitance of functionalized RGO.

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

Science.gov (United States)

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

2016-08-24

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

A simple biogenic route to rapid synthesis of Au-TiO{sub 2} nanocomposites by electrochemically active biofilms

Energy Technology Data Exchange (ETDEWEB)

Kalathil, Shafeer; Khan, Mohammad Mansoob [Yeungnam University, School of Chemical Engineering (Korea, Republic of); Banerjee, Arghya Narayan [Yeungnam University, School of Mechanical Engineering (Korea, Republic of); Lee, Jintae; Cho, Moo Hwan, E-mail: mhcho@ynu.ac.kr [Yeungnam University, School of Chemical Engineering (Korea, Republic of)

2012-08-15

Deposition of gold on titanium dioxide (TiO{sub 2}) nanoparticles is highly beneficial for maximizing the efficiency of many photocatalytic reactions. In this study, we have reported for the first time the use of an electrochemically active biofilm (EAB) for the synthesis of Au-TiO{sub 2} nanocomposite with sodium acetate as the electron donor. The EAB acts as an electron generator for the reduction of gold ions on the surface of TiO{sub 2} nanoparticles. It was observed that the TiO{sub 2} plays not only as a support for the gold nanoparticles but also as a storage of electrons produced by the EAB within the particles. These stored electrons dramatically increase the reduction of gold ions and hence we have observed the formation of the Au-TiO{sub 2} nanocomposites within 90 min. A mechanism of the nanocomposite formation is also proposed. The as-synthesized nanocomposites were characterized by UV-Vis absorption spectroscopy to monitor the proper formation of the nanocomposites. X-ray diffraction and transmission electron microscopic analyses were performed to determine the structural and microstructural properties of the nanocomposites. High-resolution transmission electron micrographs depict the proper formation of the Au-TiO{sub 2} nanocomposites with gold nanoparticle size varying from 5 to 10 nm with an increase in the gold precursor concentration. Zeta potential measurements were used to investigate surface charges of the as-synthesized nanocomposites. This novel biogenic route represents a unique pathway for the low cost, eco-friendly, rapid, and controlled synthesis of nanostructured Au-TiO{sub 2} hybrid systems which will truly revolutionize the synthetic fields of nanocomposites.

Advances in Electrocatalysis for Energy Conversion and Synthesis of Organic Molecules.

Science.gov (United States)

Holade, Yaovi; Servat, Karine; Tingry, Sophie; Napporn, Teko W; Remita, Hynd; Cornu, David; Kokoh, K Boniface

2017-10-06

Ubiquitous electrochemistry is expected to play a major role for reliable energy supply as well as for production of sustainable fuels and chemicals. The fundamental understanding of organics-based electrocatalysis in alkaline media at the solid-liquid interface involves complex mechanisms and performance descriptors (from the electrolyte and reaction intermediates), which undermine the roads towards advance and breakthroughs. Here, we review and diagnose recently designed strategies for the electrochemical conversion of organics into electricity and/or higher-value chemicals. To tune the mysterious workings of nanocatalysts in electrochemical devices, we examine the guiding principles by which the performance of a particular electrode material is governed, thus highlighting various tactics for the development of synthesis methods for nanomaterials with specific properties. We end by examining the production of chemicals by using electrochemical methods, from selective oxidation to reduction reactions. The intricate relationship between electrode and selectivity encourages both of the communities of electrocatalysis and organic synthesis to move forward together toward the renaissance of electrosynthesis methods. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and electrochemical analysis of AlVMoO7 oxide prepared ...

Indian Academy of Sciences (India)

2018-05-16

May 16, 2018 ... solid solution and two-phase regimes. In the voltage ... LiMn2O4) [1]. Among these compounds, olivine LiFePO4, ... polyanions provide numerous metal oxidation states, struc- tural stability ... 2.1a Sol–gel synthesis (SG): In SG synthesis method, ... AlVMoO7 and confirms that only a single phase is formed.

Facile fabrication and electrochemical behaviors of Mn:ZnS nanocrystals

International Nuclear Information System (INIS)

Xie, Ruishi; Li, Yuanli; Liu, Haifeng; Guo, Baogang

2016-01-01

Here, we demonstrate the rational design and synthesis of Mn:ZnS nanocrystals with adjustable doping concentrations utilizing a facile, cost effective, and environmentally benign chemical protocol. These nanostructures were investigated as electrode materials for lithium-ion batteries. Compared with pristine ZnS nanocrystals, the Mn:ZnS nanocrystals exhibit significantly improved electrochemical performances in terms of specific capacity and cycling performance. The Mn:ZnS nanocrystal sample with doping concentration of 1 at% displays second discharge capacity of 789.9 mA h g"−"1 at a current density of 24 mA g"−"1, about 2.39 times higher than that of the pure ZnS nanocrystal. Furthermore, the Mn:ZnS nanocrystal electrodes represent much better capacity retention than that of the undoped one. The greatly improved electrochemical performances of the Mn:ZnS nanocrystal samples could be attributed to the following factors. The large specific surface area can significantly enhance structural integrity by acting as mechanical buffer, effectively alleviating the volume changes generated during the lithiation/delithiation process. The incorporation of Mn into the lattice of ZnS improves charge transfer kinetics and results in a faster Li"+ diffusion rate during the charge–discharge process. It is of great significance to incorporate guest metal ions into nanostructured materials to display especial electrochemical characteristics triggering an effective approach to improve the electrochemical properties.

Facile fabrication and electrochemical behaviors of Mn:ZnS nanocrystals

Energy Technology Data Exchange (ETDEWEB)

Xie, Ruishi [Analytical and Testing Center, Southwest University of Science and Technology, Mianyang, 621010 (China); Li, Yuanli, E-mail: yuanlyl@foxmail.com [Department of Materials, Southwest University of Science and Technology, Mianyang, 621010 (China); Liu, Haifeng; Guo, Baogang [Analytical and Testing Center, Southwest University of Science and Technology, Mianyang, 621010 (China)

2016-07-05

Here, we demonstrate the rational design and synthesis of Mn:ZnS nanocrystals with adjustable doping concentrations utilizing a facile, cost effective, and environmentally benign chemical protocol. These nanostructures were investigated as electrode materials for lithium-ion batteries. Compared with pristine ZnS nanocrystals, the Mn:ZnS nanocrystals exhibit significantly improved electrochemical performances in terms of specific capacity and cycling performance. The Mn:ZnS nanocrystal sample with doping concentration of 1 at% displays second discharge capacity of 789.9 mA h g{sup −1} at a current density of 24 mA g{sup −1}, about 2.39 times higher than that of the pure ZnS nanocrystal. Furthermore, the Mn:ZnS nanocrystal electrodes represent much better capacity retention than that of the undoped one. The greatly improved electrochemical performances of the Mn:ZnS nanocrystal samples could be attributed to the following factors. The large specific surface area can significantly enhance structural integrity by acting as mechanical buffer, effectively alleviating the volume changes generated during the lithiation/delithiation process. The incorporation of Mn into the lattice of ZnS improves charge transfer kinetics and results in a faster Li{sup +} diffusion rate during the charge–discharge process. It is of great significance to incorporate guest metal ions into nanostructured materials to display especial electrochemical characteristics triggering an effective approach to improve the electrochemical properties.

Control of electro-chemical processes using energy harvesting materials and devices.

Science.gov (United States)

Zhang, Yan; Xie, Mengying; Adamaki, Vana; Khanbareh, Hamideh; Bowen, Chris R

2017-12-11

Energy harvesting is a topic of intense interest that aims to convert ambient forms of energy such as mechanical motion, light and heat, which are otherwise wasted, into useful energy. In many cases the energy harvester or nanogenerator converts motion, heat or light into electrical energy, which is subsequently rectified and stored within capacitors for applications such as wireless and self-powered sensors or low-power electronics. This review covers the new and emerging area that aims to directly couple energy harvesting materials and devices with electro-chemical systems. The harvesting approaches to be covered include pyroelectric, piezoelectric, triboelectric, flexoelectric, thermoelectric and photovoltaic effects. These are used to influence a variety of electro-chemical systems such as applications related to water splitting, catalysis, corrosion protection, degradation of pollutants, disinfection of bacteria and material synthesis. Comparisons are made between the range harvesting approaches and the modes of operation are described. Future directions for the development of electro-chemical harvesting systems are highlighted and the potential for new applications and hybrid approaches are discussed.

Synthesis and application of bismuth ferrite nanosheets supported functionalized carbon nanofiber for enhanced electrochemical detection of toxic organic compound in water samples.

Science.gov (United States)

Ramaraj, Sukanya; Mani, Sakthivel; Chen, Shen-Ming; Kokulnathan, Thangavelu; Lou, Bih-Show; Ali, M Ajmal; Hatamleh, A A; Al-Hemaid, Fahad M A

2018-03-15

Recently, the multiferroic material has fabulous attention in numerous applications owing to its excellent electronic conductivity, unique mechanical property, and higher electrocatalytic activity, etc. In this paper, we reported that the synthesis of bismuth ferrite (BiFeO 3 ) nanosheets integrated functionalized carbon nanofiber (BiFeO 3 NS/F-CNF) nanocomposite using a simple hydrothermal technique. Herein, the structural changes and crystalline property of prepared BiFeO 3 NS/F-CNF nanocomposite were characterized using Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). From this detailed structural evolution, the formation of nanosheets like BiFeO 3 and its nanocomposite with F-CNF were scrutinized and reported. Furthermore, the as-prepared BiFeO 3 NS/F-CNF nanocomposite modified glassy carbon electrode (GCE) was applied for electrochemical detection of catechol (CC). As expected, BiFeO 3 NS/F-CNF/GCE shows excellent electrocatalytic activity as well as 3.44 (F-CNF/GCE) and 7.92 (BiFeO 3 NS/GCE) fold higher electrochemical redox response for CC sensing. Moreover, the proposed sensor displays a wide linear range from 0.003 to 78.02 µM with a very low detection limit of 0.0015 µM. In addition, we have validated the real-time application of our developed CC sensor in different water samples. Copyright © 2017 Elsevier Inc. All rights reserved.

On the mechanism of electrochemical ammonia synthesis on the Ru catalyst.

Science.gov (United States)

Back, Seoin; Jung, Yousung

2016-04-07

We theoretically investigate the electrochemical N2 reduction reaction (NRR) mechanism to produce NH3 on the Ru catalyst. All possible N-N dissociation steps during the reduction processes were evaluated along with the conventional associative and dissociative pathways. Based on the calculated free energy diagrams, it is revealed that the kinetically facile intermediate dissociative pathways during the NRR require a thermodynamic limiting potential (-0.71 V) similar to the associative pathway (-0.68 V), although the initial dissociative pathway as in the Haber-Bosch process has a substantial kinetic barrier for the N-N bond dissociation. The competitive hydrogen evolution is found to be a major hurdle for achieving a high efficiency for the electrochemical nitrogen reduction. In the low overpotential region, the hydrogen adsorption is thermodynamically more favorable than the protonation of N2, thereby reducing the number of active sites for the N2 activation. A comparison of free energies in the presence of different H-coverages on the Ru further demonstrates that the H-coverage can significantly increase the energy barrier for the first protonation of N2, resulting in a change of the potential determining step and an increase in the overpotentials.

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

Science.gov (United States)

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

2014-09-01

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

Synthesis of highly faceted multiply twinned gold nanocrystals stabilized by polyoxometalates

International Nuclear Information System (INIS)

Yuan Junhua; Chen Yuanxian; Han Dongxue; Zhang Yuanjian; Shen Yanfei; Wang Zhijuan; Niu Li

2006-01-01

A novel and facile chemical synthesis of highly faceted multiply twinned gold nanocrystals is reported. The gold nanocrystals are hexagonal in transmission electron microscopy and icosahedral in scanning electron microscopy. Phosphotungstic acid (PTA), which was previously reduced, serves as a reductant and stabilizer for the synthesis of gold nanocrystals. The PTA-gold nanocomposites are quite stable in aqueous solutions, and electrochemically active towards the hydrogen evolution reaction

Synthesis of polyaniline/ZrO 2 nanocomposites and their ...

Indian Academy of Sciences (India)

Home; Journals; Bulletin of Materials Science; Volume 39; Issue 3. Synthesis of polyaniline/ZrO 2 nanocomposites and their performance in AC conductivity and electrochemical supercapacitance. B P PRASANNA D N AVADHANI H B MURALIDHARA K CHAITRA VINNY ROSE THOMAS M REVANASIDDAPPA N ...

Synthesis and Microstructural Characterization of Manganese Oxide Electrodes for Application as Electrochemical Supercapacitors

Science.gov (United States)

Babakhani, Banafsheh

The aim of this thesis work was to synthesize Mn-based oxide electrodes with high surface area structures by anodic electrodeposition for application as electrochemical capacitors. Rod-like structures provide large surface areas leading to high specific capacitances. Since templated electrosynthesis of rods is not easy to use in practical applications, it is more desirable to form rod-like structures without using any templates. In this work, Mn oxide electrodes with rod-like structures (˜1.5 µm in diameter) were synthesized from a solution of 0.01 M Mn acetate under galvanostatic control without any templates, on Au coated Si substrates. The electrochemical properties of the synthesized nanocrystalline electrodes were investigated to determine the effect of morphology, chemistry and crystal structure on the corresponding electrochemical behavior of Mn oxide electrodes. Mn oxides prepared at different current densities showed a defective antifluoritetype crystal structure. The rod-like Mn oxide electrodes synthesized at low current densities (5 mAcm.2) exhibited a high specific capacitance due to their large surface areas. Also, specific capacity retention after 250 cycles in an aqueous solution of 0.5 M Na2SO4 at 100 mVs -1 was about 78% of the initial capacity (203 Fg-1 ). To improve the electrochemical capacitive behavior of Mn oxide electrodes, a sequential approach and a one-step method were adopted to synthesize Mn oxide/PEDOT electrodes through anodic deposition on Au coated Si substrates from aqueous solutions. In the former case, free standing Mn oxide rods (about 10 µm long and less than 1.5 µm in diameter) were first synthesized, then coated by electro-polymerization of a conducting polymer (PEDOT) giving coaxial rods. The one-step, co-electrodeposition method produced agglomerated Mn oxide/PEDOT particles. The electrochemical behavior of the deposits depended on the morphology and crystal structure of the fabricated electrodes, which were affected

Combustion Synthesis Of Ultralow-density Nanoporous Gold Foams

Energy Technology Data Exchange (ETDEWEB)

Tappan, Bruce C [Los Alamos National Laboratory; Mueller, Alex H [Los Alamos National Laboratory; Steiner, Stephen A [Los Alamos National Laboratory; Luther, Erik P [Los Alamos National Laboratory

2008-01-01

A new synthetic pathway for producing nanoporous gold monoliths through combustion synthesis from Au bistetrazoJeamine complexes has been demonstrated. Applications of interest for Au nanofoams include new substrates for nanoparticle-mediated catalysis, embedded antennas, and spectroscopy. Integrated support-and-catalystin-one nanocomposites prepared through combustion synthesis of mixed AuBTA/metal oxide pellets would also be an interesting technology approach for low-cost in-line catalytic conversion media. Furthermore, we envision preparation of ultrahigh surface area gold electrodes for application in electrochemical devices through this method.

Facile electrochemical synthesis of tellurium nanorods and their photoconductive properties

Energy Technology Data Exchange (ETDEWEB)

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

2012-10-15

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

Applications of Ionic Liquids in Electrochemical Sensors and Biosensors

Directory of Open Access Journals (Sweden)

Virendra V. Singh

2012-01-01

Full Text Available Ionic liquids (ILs are salt that exist in the liquid phase at and around 298 K and are comprised of a bulky, asymmetric organic cation and the anion usually inorganic ion but some ILs also with organic anion. ILs have attracted much attention as a replacement for traditional organic solvents as they possess many attractive properties. Among these properties, intrinsic ion conductivity, low volatility, high chemical and thermal stability, low combustibility, and wide electrochemical windows are few. Due to negligible or nonzero volatility of these solvents, they are considered “greener” for the environment as they do not evaporate like volatile organic compounds (VOCs. ILs have been widely used in electrodeposition, electrosynthesis, electrocatalysis, electrochemical capacitor, lubricants, plasticizers, solvent, lithium batteries, solvents to manufacture nanomaterials, extraction, gas absorption agents, and so forth. Besides a brief discussion of the introduction, history, and properties of ILs the major purpose of this review paper is to provide an overview on the advantages of ILs for the synthesis of conducting polymer and nanoparticle when compared to conventional media and also to focus on the electrochemical sensors and biosensors based on IL/composite modified macrodisk electrodes. Subsequently, recent developments and major strategies for enhancing sensing performance are discussed.

The fractal nature materials microstructure influence on electrochemical energy sources

Directory of Open Access Journals (Sweden)

Mitić V.V.

2015-01-01

Full Text Available With increasing of the world energy crisis, research for new, renewable and alternative energy sources are in growth. The focus is on research areas, sometimes of minor importance and applications, where the different synthesis methods and microstructure properties optimization, performed significant improvement of output materials’ and components’ electro-physical properties, which is important for higher energy efficiency and in the electricity production (batteries and battery systems, fuel cells and hydrogen energy contribution. Also, the storage tanks capacity improvement, for the energy produced on such way, which is one of the most important development issues in the energy sphere, represents a very promising research and application area. Having in mind, the results achieved in the electrochemical energy sources field, especially electrolyte development, these energy sources, materials fractal nature optimization analysis contribution, have been investigated. Based on materials fractal structure research field, particularly electronic materials, we have performed microstructure influence parameters research in electrochemistry area. We have investigated the Ho2O3 concentration influence (from 0.01wt% to 1wt% and sintering temperature (from 1320°C to 1380°C, as consolidation parameters, and thus, also open the electrochemical function fractalization door and in the basic thermodynamic parameters the fractal correction introduced. The fractal dimension dependence on additive concentration is also investigated. [Projekat Ministarstva nauke Republike Srbije, br. 172057: Directed synthesis, structure and properties of multifunctional materials

Polypyrrole–titanium(IV) doped iron(III) oxide nanocomposites: Synthesis, characterization with tunable electrical and electrochemical properties

International Nuclear Information System (INIS)

Nandi, Debabrata; Ghosh, Arup Kumar; Gupta, Kaushik; De, Amitabha; Sen, Pintu; Duttachowdhury, Ankan; Ghosh, Uday Chand

2012-01-01

Highlights: ► Synthesis and characterization of polymer nanocomposite based on titanium doped iron(III) oxide. ► Electrical conductivity increased 100 times in composite with respect to polymer. ► Electrochemical capacitance of polymer composites increased with nanooxide content. ► Thermal stability of the polymer enhanced with nano oxide content. -- Abstract: Titanium(IV)-doped synthetic nanostructured iron(III) oxide (NITO) and polypyrrole (PPy) nanocomposites was fabricated by in situ polymerization using FeCl 3 as initiator. The polymer nanocomposites (PNCs) and pure NITO were characterized by X-ray diffraction, Föurier transform infrared spectroscopy, scanning electron microscopy, electron dispersive X-ray spectroscopy, transmission electron microscopy, etc. Thermo gravimetric and differential thermal analyses showed the enhancement of thermal stability of PNCs than the pure polymer. Electrical conductivity of the PNCs had increased significantly from 0.793 × 10 −2 S/cm to 0.450 S/cm with respect to the PPy, and that had been explained by 3-dimensional variable range hopping (VRH) conduction mechanisms. In addition, the specific capacitance of PNCs had increased from 147 F/g to 176 F/g with increasing NITO content than that of pure NITO (26 F/g), presumably due to the growing of mesoporous structure with increasing NITO content in PNCs which reduced the charge transfer resistance significantly.

Electrochemical Performance of LixMn2-yFeyO4-zClz Synthesized Through In-Situ Glycine Nitrate Combustion

Science.gov (United States)

2016-06-13

Electrochemical Performance of LixMn2-yFeyO4-zClz Synthesized Through In-Situ Glycine Nitrate Combustion Ashley L. Ruth, Paula C. Latorre, and...sites as well as the formation of Mn3+ ions via the Jahn- Teller effect. The use of the glycine nitrate combustion synthesis produces small particles at...advantage of submicron ceramic synthesis, namely the glycine nitrate combustion process (GNP), we propose the capability for in-situ B-site doping

Studies on room temperature electrochemical oxidation and its effect on the transport properties of TBCCO films

International Nuclear Information System (INIS)

Shirage, P M; Shivagan, D D; Pawar, S H

2004-01-01

A novel room temperature electrochemical process for the synthesis of single-phase Tl 2 Ba 2 Ca 2 Cu 3 O 10 (TBCCO/Tl-2223) superconducting films has been developed. Electrochemical parameters were optimized by studying linear sweep voltammetry (LSV), cyclic voltammetry (CV) and chronoamperometry (CA) for the deposition of Tl-Ba-Ca-Cu alloy at room temperature. The superconducting films of the TBCCO were obtained by two oxidation techniques. In the first technique, the electrodeposited Tl-Ba-Ca-Cu alloyed films were oxidized at various temperatures in flowing oxygen atmosphere. In the second technique, stoichiometric electrocrystallization to get Tl 2 Ba 2 Ca 2 Cu 3 O 10 (Tl-2223) was completed by electrochemically intercalating oxygen species into Tl-Ba-Ca-Cu alloy at room temperature for various lengths of time. The oxygen content in the samples was varied by varying the electrochemical oxidation period, and the changes in the crystal structure, superconducting transition temperature (T c ) and critical current density (J c ) were recorded. The high temperature furnace oxidation technique was replaced by the room temperature electrochemical oxidation technique. The dependence of superconducting parameters on oxygen content is correlated with structure-property relations

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-02-11

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2011-05-06

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

Synthesis, spectroscopic and electrochemical performance of pasted β-nickel hydroxide electrode in alkaline electrolyte

Science.gov (United States)

Shruthi, B.; Bheema Raju, V.; Madhu, B. J.

2015-01-01

β-Nickel hydroxide (β-Ni(OH)2) was successfully synthesized using precipitation method. The structure and property of the β-Ni(OH)2 were characterized by X-ray diffraction (XRD), Fourier Transform infra-red (FT-IR), Raman spectra and thermal gravimetric-differential thermal analysis (TG-DTA). The results of the FTIR spectroscopy and TG-DTA studies indicate that the β-Ni(OH)2 contains water molecules and anions. The microstructural and composition studies have been performed using Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray (EDX) analysis. A pasted-type electrode is prepared using β-Ni(OH)2 powder as the active material on a nickel sheet as a current collector. Cyclic voltammetry (CV) and Electrochemical impedance spectroscopy (EIS) studies were performed to evaluate the electrochemical performance of the β-Ni(OH)2 electrode in 6 M KOH electrolyte. CV curves showed a pair of strong redox peaks as a result of the Faradaic redox reactions of β-Ni(OH)2. The proton diffusion coefficient (D) for the present β-Ni(OH)2 electrode material is found to be 1.44 × 10-12 cm2 s-1. Further, electrochemical impedance studies confirmed that the β-Ni(OH)2 electrode reaction processes are diffusion controlled.

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

KAUST Repository

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

2013-01-01

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

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

KAUST Repository

Shahid, Muhammad

2013-05-01

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

Pyro-Synthesis of Functional Nanocrystals

OpenAIRE

Gim, Jihyeon; Mathew, Vinod; Lim, Jinsub; Song, Jinju; Baek, Sora; Kang, Jungwon; Ahn, Docheon; Song, Sun-Ju; Yoon, Hyeonseok; Kim, Jaekook

2012-01-01

Despite nanomaterials with unique properties playing a vital role in scientific and technological advancements of various fields including chemical and electrochemical applications, the scope for exploration of nano-scale applications is still wide open. The intimate correlation between material properties and synthesis in combination with the urgency to enhance the empirical understanding of nanomaterials demand the evolution of new strategies to promising materials. Herein we introduce a ra...

Electrolytes and Electrodes for Electrochemical Synthesis of Ammonia

DEFF Research Database (Denmark)

Lapina, Alberto

In order to make Denmark independent of fossil fuels by 2050 the share of renewable energy in electricity production, in particular wind energy, is expected to increase significantly. Since the power output of renewable energy sources heavily fluctuates over time there is a pressing need to find...... technology is based on the Haber-Bosch process, which is energy intensive and requires large-scale plants. One possible way to produce ammonia from sustainable electricity, nitrogen and hydrogen/water is using an electrochemical cell. This thesis studies a number of electrolytes and electrocatalysts...... state proton conductors are briefly reviewed and defect chemistry and partial conductivities of Y-doped BaZrO3-BaCeO3 solid solutions are studied as a function of temperature, pH2O and chemical compositions by means of defect chemistry modelling. BaCe0.2Zr0.6Y0.2O2.9 (BCZY26) is chosen as electrolyte...

Electrochemical promotion of catalytic reactions with Pt/C (or Pt/Ru/C)//PBI catalysts

DEFF Research Database (Denmark)

Petrushina, Irina; Bjerrum, Niels; Bandur, Viktor

2007-01-01

The paper is an overview of the results of the investigation on electrochemical promotion of three catalytic reactions: methane oxidation with oxygen, NO reduction with hydrogen at 135 degrees C and Fischer-Tropsch synthesis (FTS) at 170 degrees C in the [CH4/O-2(or NO/H-2 or CO/H-2)/Ar//Pt(or Pt....../Ru)//PBI(H3PO4)/H-2, Ar] fuel cell. It has been shown that the partial methane oxidation to C2H2 and the C-2 selectivity were electrochemically promoted by the negative catalyst polarization. This was also the case in NO reduction with hydrogen for low NO and H-2 partial pressures. In both cases the catalytic...... reactions have been promoted by the electrochemically produced hydrogen. It has been found that the NO reduction with hydrogen on the Pt/PBI strongly depends on NO and hydrogen partial pressures in the working gas mixture. At higher NO and H-2 partial pressures the catalysis is promoted...

Synthesis of graphene oxide through different oxidation degrees for solar cells

Science.gov (United States)

Zhang, Xiaoshan; Wang, Huan; Huang, Tianjiao; Wen, Lingling; Zhou, Liya

2018-03-01

Graphene is known as an electro-chemical material and widely used in electro-chemical devices, especially in solar cell. Decreasing the thickness of the layer is a critical way to improve the electrochemical property of solar cells as far as possible. Among the various oxidation approaches, presented herein is a facile approach, which is easier, less cost and more effective, environmental benign with the greener processing and without any requirement for post purification, towards the synthesis of graphene oxide (GO) with different oxidation degrees by potassium ferrate (K2FeO4). A modified method using less amount of oxidizing agent is reported herein. It is the pretreatment of the synthesis of graphite, which maintains the thermal cycle of the system. This novel reports to compound GO with controlled oxidation degrees can not only increase the quantity of oxygen-containing functional groups on GO surface, increase space between graphene oxide layer and facilitate the dispersion of graphene in aqueous solution. Thus, the modified method shows prospect for large-scale production of graphene oxide and its novel application, in addition to its derivative and market potential for solar cells.

Facile synthesis of polypyrrole nanofiber and its enhanced electrochemical performances in different electrolytes

Directory of Open Access Journals (Sweden)

C. K. Das

2012-12-01

Full Text Available A porous nanocomposite based on polypyrrole (PPy and sodium alginate (SA has been synthesized by easy, inexpensive, eco-friendly method. As prepared nanocomposite showed fibrillar morphology in transmission electron microscopic (TEM analysis. The average diameter of ~100 nm for the nanofibers was observed from scanning electron microscopic (SEM analysis. As prepared nanofiber, was investigated as an electrode material for supercapacitor application in different aqueous electrolyte solutions. PPy nanofiber showed enhanced electrochemical performances in 1M KCl solution as compared to 1M Na2SO4 solution. Maximum specific capacitance of 284 F/g was found for this composite in 1 M KCl electrolyte. It showed 76% specific capacitance retention after 600 cycles in 1 M KCl solution. Electrochemical Impedance Spectra showed moderate capacitive behavior of the composite in both the electrolytes. Further PPy nanofiber demonstrated higher thermal stability as compared to pure PPy.

Facile synthesis of a silver nanoparticles/polypyrrole nanocomposite for non-enzymatic glucose determination.

Science.gov (United States)

Poletti Papi, Maurício A; Caetano, Fabio R; Bergamini, Márcio F; Marcolino-Junior, Luiz H

2017-06-01

The present work describes the synthesis of a new conductive nanocomposite based on polypyrrole (PPy) and silver nanoparticles (PPy-AgNP) based on a facile reverse microemulsion method and its application as a non-enzymatic electrochemical sensor for glucose detection. Focusing on the best sensor performance, all experimental parameters used in the synthesis of nanocomposite were optimized based on its electrochemical response for glucose. Characterization of the optimized material by FT-IR, cyclic voltammetry, and DRX measurements and TEM images showed good monodispersion of semispherical Ag nanoparticles capped by PPy structure, with size average of 12±5nm. Under the best analytical conditions, the proposed sensor exhibited glucose response in linear dynamic range of 25 to 2500μmolL -1 , with limit of detection of 3.6μmolL -1 . Recovery studies with human saliva samples varying from 99 to 105% revealed the accuracy and feasibility of a non-enzymatic electrochemical sensor for glucose determination by easy construction and low-cost. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis, spectroscopic characterization and pH dependent photometric and electrochemical fate of Schiff bases.

Science.gov (United States)

Rauf, Abdur; Shah, Afzal; Abbas, Saghir; Rana, Usman Ali; Khan, Salah Ud-Din; Ali, Saqib; Zia-Ur-Rehman; Qureshi, Rumana; Kraatz, Heinz-Bernhard; Belanger-Gariepy, Francine

2015-03-05

A new Schiff base, 1-((4-bromophenylimino) methyl) naphthalen-2-ol (BPIMN) was successfully synthesized and characterized by (1)H NMR, (13)C NMR, FTIR and UV-Vis spectroscopy. The results were compared with a structurally related Schiff base, 1-((4-chlorophenylimino) methyl) naphthalen-2-ol (CPIMN). The photometric and electrochemical fate of BPIMN and CPIMN was investigated in a wide pH range. The experimental findings were supported by quantum mechanical approach. The redox mechanistic pathways were proposed on the basis of results obtained electrochemical techniques. Moreover, pH dependent UV-Vis spectroscopy of BPIMN and CPIMN was carried out and the appearance of isosbestic points indicated the existence of these compounds in different tautomeric forms. Copyright © 2014 Elsevier B.V. All rights reserved.

Novel electrochemical redox-active species: one-step synthesis of polyaniline derivative-Au/Pd and its application for multiplexed immunoassay

Science.gov (United States)

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.

Effect of reducing agents on low-temperature synthesis of nanostructured LiFePO4

Science.gov (United States)

Kulka, Andrzej; Walczak, Katarzyna; Zając, Wojciech; Molenda, Janina

2017-09-01

Simple co-precipitation synthesis procedure yielding nanometric LiFePO4 with enhanced electrochemical properties without any post-synthesis heat treatment is presented. XRD, SEM and TEM analysis of the obtained powders revealed platelet crystallites and well crystalized bulk structure. Effective way of decreasing amount of Fe3+ containing phases by addition of reducing agents (KI, (NH4)2S2O3, glucose and the atmosphere of 5%H2-95%Ar) during low-temperature (107 °C) synthesis is described. The traditional analytical chemistry methods or the Mӧssbauer spectroscopy methods revealed that utilization of selected reducing agents diminished Fe3+ concentration from 25 to 12 at%. The constructed cells with optimized LiFePO4 as a cathode material showed superior electrochemical performances, including high reversible capacity up to 162 mAh/g at C/10 current discharge rate, flat voltage plateau with a value close to 3.45 V vs. Li0/+.

Effect of calcination temperature on microstructure and electrochemical performance of lithium-rich layered oxide cathode materials

International Nuclear Information System (INIS)

Ma, Quanxin; Peng, Fangwei; Li, Ruhong; Yin, Shibo; Dai, Changsong

2016-01-01

Highlights: • A series of Li-rich layered oxide cathode materials (Li_1_._2Mn_0_._5_6Ni_0_._1_6Co_0_._0_8O_2) were successfully synthesized via a two-step synthesis method. • The effects of calcination temperature on the cathode materials were researched in detail. • A well-crystallized layered structure was obtained as the calcination temperature increased. • The samples calcined in a range of 850–900 °C exhibited excellent electrochemical performance. - Abstract: Lithium-rich layered oxide cathode materials (Li_1_._2Mn_0_._5_6Ni_0_._1_6Co_0_._0_8O_2 (LLMO)) were synthesized via a two-step synthesis method involving co-precipitation and high-temperature calcination. The effects of calcination temperature on the cathode materials were studied in detail. Structural and morphological characterizations revealed that a well-crystallized layered structure was obtained at a higher calcination temperature. Electrochemical performance evaluation revealed that a cathode material obtained at a calcination temperature of 850 °C delivered a high initial discharge capacity of 266.8 mAh g"−"1 at a 0.1 C rate and a capacity retention rate of 95.8% after 100 cycles as well as excellent rate capability. Another sample calcinated at 900 °C exhibited good cycling stability. It is concluded that the structural stability and electrochemical performance of Li-rich layered oxide cathode materials were strongly dependent on calcination temperatures. The results suggest that a calcination temperature in a range of 850–900 °C could promote electrochemical performance of this type of cathode materials.

Effect of calcination temperature on microstructure and electrochemical performance of lithium-rich layered oxide cathode materials

Energy Technology Data Exchange (ETDEWEB)

Ma, Quanxin; Peng, Fangwei; Li, Ruhong; Yin, Shibo; Dai, Changsong, E-mail: changsd@hit.edu.cn

2016-11-15

Highlights: • A series of Li-rich layered oxide cathode materials (Li{sub 1.2}Mn{sub 0.56}Ni{sub 0.16}Co{sub 0.08}O{sub 2}) were successfully synthesized via a two-step synthesis method. • The effects of calcination temperature on the cathode materials were researched in detail. • A well-crystallized layered structure was obtained as the calcination temperature increased. • The samples calcined in a range of 850–900 °C exhibited excellent electrochemical performance. - Abstract: Lithium-rich layered oxide cathode materials (Li{sub 1.2}Mn{sub 0.56}Ni{sub 0.16}Co{sub 0.08}O{sub 2} (LLMO)) were synthesized via a two-step synthesis method involving co-precipitation and high-temperature calcination. The effects of calcination temperature on the cathode materials were studied in detail. Structural and morphological characterizations revealed that a well-crystallized layered structure was obtained at a higher calcination temperature. Electrochemical performance evaluation revealed that a cathode material obtained at a calcination temperature of 850 °C delivered a high initial discharge capacity of 266.8 mAh g{sup −1} at a 0.1 C rate and a capacity retention rate of 95.8% after 100 cycles as well as excellent rate capability. Another sample calcinated at 900 °C exhibited good cycling stability. It is concluded that the structural stability and electrochemical performance of Li-rich layered oxide cathode materials were strongly dependent on calcination temperatures. The results suggest that a calcination temperature in a range of 850–900 °C could promote electrochemical performance of this type of cathode materials.

Synthesis and Electrochemical Properties of Fe-doped V6O13 as Cathode Material for Lithium-ion Battery

Directory of Open Access Journals (Sweden)

YUAN Qi

2018-01-01

Full Text Available Fe-doped V6O13 was synthesized via a facile hydrothermal method after preparing precursor in order to improve the discharge capacity and cycle performance of V6O13 cathode material at high-lithium state. XRD, SEM and XPS were employed to characterize the phase, morphology and valence of the Fe-doped V6O13. Meanwhile, the electrochemical performance was analyzed and researched. Different morphologies and electrochemical performances of Fe-doped V6O13 were obtained via doping different contents of Fe3+ ion. The sample 0.02 presented the largest thickness of nanosheets (the thickness of 600-900nm and clearance between layers. The Fe-doped V6O13 has a better electrochemical performance than that of pure V6O13. The sample 0.02 exhibits the best electrochemical performance, the initial discharge specific capacity is 433mAh·g-1 and the capacity retention is 47.1% after 100 cycles.

Electrochemical biosensors

CERN Document Server

Cosnier, Serge

2015-01-01

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

Plasma-Assisted Synthesis and Surface Modification of Electrode Materials for Renewable Energy.

Science.gov (United States)

Dou, Shuo; Tao, Li; Wang, Ruilun; El Hankari, Samir; Chen, Ru; Wang, Shuangyin

2018-02-14

Renewable energy technology has been considered as a "MUST" option to lower the use of fossil fuels for industry and daily life. Designing critical and sophisticated materials is of great importance in order to realize high-performance energy technology. Typically, efficient synthesis and soft surface modification of nanomaterials are important for energy technology. Therefore, there are increasing demands on the rational design of efficient electrocatalysts or electrode materials, which are the key for scalable and practical electrochemical energy devices. Nevertheless, the development of versatile and cheap strategies is one of the main challenges to achieve the aforementioned goals. Accordingly, plasma technology has recently appeared as an extremely promising alternative for the synthesis and surface modification of nanomaterials for electrochemical devices. Here, the recent progress on the development of nonthermal plasma technology is highlighted for the synthesis and surface modification of advanced electrode materials for renewable energy technology including electrocatalysts for fuel cells, water splitting, metal-air batteries, and electrode materials for batteries and supercapacitors, etc. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis of cadmium oxide doped ZnO nanostructures using electrochemical deposition

International Nuclear Information System (INIS)

Singh, Trilok; Pandya, D.K.; Singh, R.

2011-01-01

Research highlights: → Ternary ZnCdO alloy semiconductor nanostructures were grown using electrochemical deposition. → X-ray diffraction measurements showed that the nanostructures were of wurtzite structure and possessed a compressive stress along the c-axis direction. → The cut-off wavelength shifted from blue to red on account of the Cd incorporation in the ZnO and the average transmittance decreased by ∼31%. → The bandgap tuning for 4-16 at% Cd in the initial solution was achieved in the range of 3.08-3.32 eV (up to 0.24 eV). - Abstract: Ternary ZnCdO alloy semiconductor nanostructures were grown using electrochemical deposition. Crystalline nanostructures/nanorods with cadmium concentration ranging from 4 to 16 at% in the initial solution were electrodeposited on tin doped indium oxide (ITO) conducting glass substrates at a constant cathodic potential -0.9 V and subsequently annealed in air at 300 deg. C. X-ray diffraction measurements showed that the nanostructures were of wurtzite structure and possessed a compressive stress along the c-axis direction. The elemental composition of nanostructures was confirmed by energy dispersive spectroscopy (EDS). ZnO nanostructures were found to be highly transparent and had an average transmittance of 85% in the visible range of the spectrum. After the incorporation of Cd content into ZnO the average transmittance decreased and the bandgap tuning was also achieved.

Synthesis and electrochemical performance of polyaniline-MnO2 nanowire composites for supercapacitors

Science.gov (United States)

Chen, Ling; Song, Zhaoxia; Liu, Guichang; Qiu, Jieshan; Yu, Chang; Qin, Jiwei; Ma, Lin; Tian, Fengqin; Liu, Wei

2013-02-01

Polyaniline-MnO2 nanowire (PANI-MNW) composites were prepared by in situ chemical oxidative polymerization of aniline monomer in a suspension of MnO2 nanowires. The structure and morphology of the PANI-MNW composites were characterized by powder X-ray diffraction (XRD) and scanning electron microscopy (SEM). Their electrochemical properties were investigated using cyclic voltammetry, galvanostatic charge-discharge and electrochemical impedance spectroscopy in 1 mol/L KOH electrolyte. The PANI-MNW composites show significantly better specific capacity and redox performance in comparison to the untreated MnO2 nanowires. The enhanced properties can be mainly attributed to the composite structure wherein high porosity is created between MnO2 nanowires and PANI during the process of fabricating the PANI-MNW nanocomposites. A specific capacitance as high as 256 F/g is obtained at a current density of 1 A/g for PANI-MNW-5, and the composite also shows a good cyclic performance and coulomb efficiency.

Facile synthesis and photo electrochemical performance of SnSe thin films

Science.gov (United States)

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

2018-05-01

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

Novel synthesis of methoxymethyl benzene by electrochemical coupling reaction of toluene with methanol in ionic liquid media.

Science.gov (United States)

Chen, Fengtao; Wang, Bo; Ma, Hongzhu

2009-06-15

An ionic liquid (1-butyl-3-methylimidazolium dibutyl phosphate) was prepared and characterized by cyclic voltammogram (CV) and Fourier transform infrared spectrometer (FT-IR). The ionic liquid exhibited good catalytic activity for the electrochemical reaction of toluene with methanol assisted with a pair of porous graphite plane electrodes and product yield higher than 56% was observed. In addition, the electrochemical process was detected by UV-vis spectrum and the products were analyzed by gas chromatography/mass spectrometry (GC/MS). According to the experimental results, a possible free radical reaction mechanism was proposed. It may be concluded that a simply and feasible electrochemical coupling reaction at room temperature and atmospheric pressure may be possible. Compared with methyl tert-butyl ether (MTBE), the main product (methoxymethyl benzene) used as booster to improve fuel combustion was also studied.

Synthesis of ZnCo{sub 2}O{sub 4} microspheres with Zn{sub 0.33}Co{sub 0.67}CO{sub 3} precursor and their electrochemical performance

Energy Technology Data Exchange (ETDEWEB)

Lu, Lin; Xu, Shan; Luo, Zhaohui; Wang, Shiquan, E-mail: wsqhao@126.com; Li, Guohua; Feng, Chuanqi [Hubei University, Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Ministry-of-Education Key Laboratory for Synthesis and Applications of Organic Functional Molecules (China)

2016-07-15

Zn{sub 0.33}Co{sub 0.67}CO{sub 3} (ZCCO) microspheres are fabricated by a facile solvothermal method at different temperatures, and ZnCo{sub 2}O{sub 4} (ZCO) microspheres were further obtained by pyrolysis of the relative ZCCO precursors at 450 °C. All samples were characterized by X-ray diffractometer, Fourier transform infrared spectra, thermogravimetric, scanning electron microscopy, transmission electron microscopy and Brunauer–Emmett–Teller (BET). Their electrochemical properties were investigated as the anode materials for the lithium-ion battery applications. The results showed that both the ZCCO and ZCO electrodes possess high specific capacities, and the synthesis temperature greatly influenced their performances. Compared with the synthesized of 180 °C, the synthesized of 200 °C (ZCCO-200) exhibited higher discharge capacity (1530 mAh g{sup −1}) and better rate performance with the reversible capacity of 876 mAh g{sup −1} after 70 cycles under the voltage range of 0.01–3.0 V at the current density of 100 mA g{sup −1}. The as-obtained ZCO microspheres from the pyrolysis of ZCCO-200 also exhibited higher discharge capacity of 1416 mAh g{sup −1} and better cycling stability (741 mAh g{sup −1} after 70 cycles) than that for the microspheres from the pyrolysis of ZCO-180, indicating that the electrochemical properties of ZCO may be related to the electrochemical performance of ZCCO. Our present work suggested that both the ZCCO and ZCO microspheres can be promising candidates as novel anode materials for lithium-ion battery applications.

Self-assembled Ti3C2Tx/SCNT composite electrode with improved electrochemical performance for supercapacitor.

Science.gov (United States)

Fu, Qishan; Wang, Xinyu; Zhang, Na; Wen, Jing; Li, Lu; Gao, Hong; Zhang, Xitian

2018-02-01

Two-dimensional titanium carbide has gained considerable attention in recent years as an electrode material for supercapacitors due to its high melting point, good electrical conductivity, hydrophilicity and large electrochemically active surfaces. However, the irreversible restacking during synthesis restricts its development and practical applications. Here, Ti 3 C 2 T x /SCNT self-assembled composite electrodes were rationally designed and successfully synthesized by introducing single-walled carbon nanotubes (SCNTs) as interlayer spacers to decrease the restacking of the Ti 3 C 2 T x sheets during the synthesis process. SCNTs can not only increase the specific surface area as well as the interlayer space of the Ti 3 C 2 T x electrode, but also increase the accessible capability of electrolyte ions, and thus it improved the electrochemical performance of the electrode. The as-prepared Ti 3 C 2 T x /SCNT self-assembled composite electrode achieved a high areal capacitance of 220mF/cm 2 (314F/cm 3 ) and a remarkable capacitance retention of 95% after 10,000cycles. Copyright © 2017 Elsevier Inc. All rights reserved.

Nanostructured Mo-based electrode materials for electrochemical energy storage.

Science.gov (United States)

Hu, Xianluo; Zhang, Wei; Liu, Xiaoxiao; Mei, Yueni; Huang, Yunhui

2015-04-21

The development of advanced energy storage devices is at the forefront of research geared towards a sustainable future. Nanostructured materials are advantageous in offering huge surface to volume ratios, favorable transport features, and attractive physicochemical properties. They have been extensively explored in various fields of energy storage and conversion. This review is focused largely on the recent progress in nanostructured Mo-based electrode materials including molybdenum oxides (MoO(x), 2 ≤ x ≤ 3), dichalconides (MoX2, X = S, Se), and oxysalts for rechargeable lithium/sodium-ion batteries, Mg batteries, and supercapacitors. Mo-based compounds including MoO2, MoO3, MoO(3-y) (0 energy storage systems because of their unique physicochemical properties, such as conductivity, mechanical and thermal stability, and cyclability. In this review, we aim to provide a systematic summary of the synthesis, modification, and electrochemical performance of nanostructured Mo-based compounds, as well as their energy storage applications in lithium/sodium-ion batteries, Mg batteries, and pseudocapacitors. The relationship between nanoarchitectures and electrochemical performances as well as the related charge-storage mechanism is discussed. Moreover, remarks on the challenges and perspectives of Mo-containing compounds for further development in electrochemical energy storage applications are proposed. This review sheds light on the sustainable development of advanced rechargeable batteries and supercapacitors with nanostructured Mo-based electrode materials.

Synthesis And Electrochemical Characteristics Of Mechanically Alloyed Anode Materials SnS2 For Li/SnS2 Cells

Directory of Open Access Journals (Sweden)

Hong J.H.

2015-06-01

Full Text Available With the increasing demand for efficient and economic energy storage, tin disulfide (SnS2, as one of the most attractive anode candidates for the next generation high-energy rechargeable Li-ion battery, have been paid more and more attention because of its high theoretical energy density and cost effectiveness. In this study, a new, simple and effective process, mechanical alloying (MA, has been developed for preparing fine anode material tin disulfides, in which ammonium chloride (AC, referred to as process control agents (PCAs, were used to prevent excessive cold-welding and accelerate the synthesis rates to some extent. Meanwhile, in order to decrease the mean size of SnS2 powder particles and improve the contact areas between the active materials, wet milling process was also conducted with normal hexane (NH as a solvent PCA. The prepared powders were both characterized by X-ray diffraction, Field emission-scanning electron microscopeand particle size analyzer. Finally, electrochemical measurements for Li/SnS2 cells were takenat room temperature, using a two-electrode cell assembled in an argon-filled glove box and the electrolyte of 1M LiPF6 in a mixture of ethylene carbonate(EC/dimethylcarbonate (DMC/ethylene methyl carbonate (EMC (volume ratio of 1:1:1.

Electrochemical energy generation

International Nuclear Information System (INIS)

Kreysa, G.; Juettner, K.

1993-01-01

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

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

Directory of Open Access Journals (Sweden)

JIANG Chao

2016-12-01

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

Preparation of Nickel Cobalt Sulfide Hollow Nanocolloids with Enhanced Electrochemical Property for Supercapacitors Application

Science.gov (United States)

Chen, Zhenhua; Wan, Zhanghui; Yang, Tiezhu; Zhao, Mengen; Lv, Xinyan; Wang, Hao; Ren, Xiuli; Mei, Xifan

2016-01-01

Nanostructured functional materials with hollow interiors are considered to be good candidates for a variety of advanced applications. However, synthesis of uniform hollow nanocolloids with porous texture via wet chemistry method is still challenging. In this work, nickel cobalt precursors (NCP) in sub-micron sized spheres have been synthesized by a facile solvothermal method. The subsequent sulfurization process in hydrothermal system has changed the NCP to nickel cobalt sulfide (NCS) with porous texture. Importantly, the hollow interiors can be tuned through the sulfurization process by employing different dosage of sulfur source. The derived NCS products have been fabricated into supercapacitor electrodes and their electrochemical performances are measured and compared, where promising results were found for the next-generation high-performance electrochemical capacitors. PMID:27114165

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

Science.gov (United States)

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

2017-10-15

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

Hierarchical architecture of ReS_2/rGO composites with enhanced electrochemical properties for lithium-ion batteries

International Nuclear Information System (INIS)

Qi, Fei; Chen, Yuanfu; Zheng, Binjie; He, Jiarui; Li, Qian; Wang, Xinqiang; Lin, Jie; Zhou, Jinhao; Yu, Bo; Li, Pingjian; Zhang, Wanli

2017-01-01

Highlights: • The ReS_2/rGO composites have been synthesized by a facile one-pot method. • The ReS_2/rGO composites exhibit hierarchical architecture. • The ReS_2/rGO composites deliver better electrochemical performances than ReS_2. • The enhanced performance is due to porous and conductive structure of ReS_2/rGO. - Abstract: Rhenium disulfide (ReS_2), a two-dimensional (2D) semiconductor, has attracted more and more attention due to its unique anisotropic electronic, optical, mechanical properties. However, the facile synthesis and electrochemical property of ReS_2 and its composite are still necessary to be researched. In this study, for the first time, the ReS_2/reduced graphene oxide (rGO) composites have been synthesized through a facile and one-pot hydrothermal method. The ReS_2/rGO composites exhibit a hierarchical, interconnected, and porous architecture constructed by nanosheets. As anode for lithium-ion batteries, the as-synthesized ReS_2/rGO composites deliver a large initial capacity of 918 mAh g"−"1 at 0.2 C. In addition, the ReS_2/rGO composites exhibit much better electrochemical cycling stability and rate capability than that of bare ReS_2. The significant enhancement in electrochemical property can be attributed to its unique architecture constructed by nanosheets and porous structure, which can allow for easy electrolyte infiltration, efficient electron transfer, and ionic diffusion. Furthermore, the graphene with high electronic conductivity can provide good conductive passageways. The facile synthesis approach can be extended to prepare other 2D transition metal dichalcogenides semiconductors for energy storage and catalytic application.

Morphology of the porous silicon obtained by electrochemical anodization method

Science.gov (United States)

Bertel H, S. D.; Dussán C, A.; Diaz P, J. M.

2018-04-01

In this report, the dependence of porous silicon with the synthesis parameters and their correlation with the optical and morphological properties is studied. The P-type silicon-crystalline samples and orientation were prepared by electrochemical anodization and were characterized using SEM in order to know the evolution of the pore morphology. It was observed that the porosity and thickness of the samples increased with the increase of the concentration in the solution and a high pore density (70%) with a pore size between 40nm and 1.5μm.

Synthesis of iron oxides nanoparticles with very high saturation magnetization form TEA-Fe(III) complex via electrochemical deposition for supercapacitor applications

Science.gov (United States)

Elrouby, Mahmoud; Abdel-Mawgoud, A. M.; El-Rahman, Rehab Abd

2017-11-01

This work is devoted to the synthesis of magnetic iron oxides nanoparticles with very high saturation magnetization to be qualified for supercapacitor applications using, a simple electrodeposition technique. It is found that the electrochemical reduction process depends on concentration, temperature, deposition potential and the scan rate of potential. The nature of electrodeposition process has been characterized via voltammetric and chronoamperometric techniques. The morphology of the electrodeposits has been investigated using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The structure and phase content of these investigated electrodeposits have been examined and calculated. The obtained iron oxides show a high saturation magnetization (Ms) of about 229 emu g-1. The data exhibited a relation between Ms of electrodeposited iron oxide and specific capacitance. This relation exhibits that the highest Ms value of electrodeposited iron oxides gives also highest specific capacitance of about 725 Fg-1. Moreover, the electrodeposited iron oxides exhibit a very good stability. The new characteristics of the electro synthesized iron oxides at our optimized conditions, strongly qualify them as a valuable material for high-performance supercapacitor applications.

Silicon-containing polyoxadiazoles-synthesis and perspectives.

Science.gov (United States)

Bruma, Maria; Köpnick, Thomas

2005-11-30

A review is presented on those polymers which contain diphenylsilylene units and 1,3,4-oxadiazole rings either in the main chain or in the pendent groups. The synthesis of silicon-containing monomers as well as of the polyoxadiazoles based on them is described. The properties of these polymers, such as solubility, film forming ability, thermal stability, electrochemical behavior and photoluminescence properties, and their potential applications are discussed.

Na{sub 2}EDTA-assisted hydrothermal synthesis and electrochemical performance of LiFePO{sub 4} powders with rod-like and block-like morphologies

Energy Technology Data Exchange (ETDEWEB)

Wang, Juan, E-mail: juanwang168@gmail.com [Shaanxi Key Laboratory of Nanomaterials and Nanotechnology, Xi' an University of Architecture and Technology, Xi' an 710055 (China); Zheng, Siqi; Yan, Hao; Zhang, Haipeng [Shaanxi Key Laboratory of Nanomaterials and Nanotechnology, Xi' an University of Architecture and Technology, Xi' an 710055 (China); Hojamberdiev, Mirabbos [Materials and Structures Laboratory, Tokyo Institute of Technology, 4259 Nagatsuta, Midori, Yokohama, Kanagawa 226-8503 (Japan); Ren, Bing; Xu, Yunhua [Shaanxi Key Laboratory of Nanomaterials and Nanotechnology, Xi' an University of Architecture and Technology, Xi' an 710055 (China)

2015-06-15

Nano and micro-sized LiFePO{sub 4} were synthesized by disodium ethylenediamine tetraacetate (Na{sub 2}EDTA) – assisted hydrothermal synthesis method with the pH of synthesizing solution in the range from 2 to 8. The as-synthesized samples were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM) and electrochemical performance experiments. The obtained results showed that the pH of synthesizing solution played a key role in the formation of the final products with different morphologies, including rod-like and block-like structures and so on. The formation mechanism and the influence of Na{sub 2}EDTA on the morphology of LiFePO{sub 4} micro- and nanocrystals were investigated as a function of pH value. The results of electrochemical performance measurement revealed that the charge/discharge cycling characteristics of the samples were varied by tailoring their morphologies. Particularly, the block-like LiFePO{sub 4} particles with the average size of 200–600 nm present the highest initial discharge capacity of 141 mAh/g at 0.1C rate, and cycling stability of this sample is optimal among all the obtained products owing to its good diffusion properties. It also exhibits an excellent rate capability with high discharge capacities of more than 93.2 mAh/g at 5C after 80 cycles. The present study offers a simple way to synthesize and design high performance cathode materials for lithium-ion batteries by the methods of morphology control without carbon coating or doping with supervalent cations. - Highlights: • Nano and micro-sized LiFePO{sub 4} were synthesized by a hydrothermal synthesis method. • Effect of the pH of synthesizing solution on the formation of LiFePO{sub 4} was studied. • The block-like LiFePO{sub 4} particles present the highest initial discharge capacity. • The rate capability of the block-like LiFePO{sub 4} is more than 93.2 m

Synthesis and electrochemical behavior of nanostructured cauliflower-shape Co-Ni/Co-Ni oxides composites

International Nuclear Information System (INIS)

Gupta, Vinay; Kawaguchi, Toshikazu; Miura, Norio

2009-01-01

Nanostructured Co-Ni/Co-Ni oxides were electrochemically deposited onto stainless steel electrode by electrochemical method and characterized for their structural and supercapacitive properties. The SEM images indicated that the obtained Co-Ni/Co-Ni oxides had cauliflower-type nanostructure. The X-ray diffraction pattern showed the formation of Co 3 O 4 , NiO, Co and Ni. The EDX elemental mapping images indicated that Ni, Co and O are distributed uniformly. The deposited Co-Ni/Co-Ni oxides showed good supercapacitive characteristics with a specific capacitance of 331 F/g at 1 mA/cm 2 current density in 1 M KOH electrolyte. A mechanism of the formation of cauliflower-shape Co-Ni/Co-Ni oxides was proposed. A variety of promising applications in the fields such as energy storage devices and sensors can be envisioned from Co-Ni/Co-Ni oxides

Resistive Switching Characteristics in Electrochemically Synthesized ZnO Films

Directory of Open Access Journals (Sweden)

Shuhan Jing

2015-04-01

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

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

Science.gov (United States)

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.%.

Simple Synthesis and Enhanced Performance of Graphene Oxide-Gold Composites

Directory of Open Access Journals (Sweden)

Min Song

2012-01-01

Full Text Available Graphene oxide-gold composites were prepared by one-step reaction in aqueous solution, where the gold nanoparticles were deposited on the graphene oxide during their synthesis process. Transmission electron morphology, X-ray diffraction, Roman spectra, and UV-Vis absorption spectra were used to characterize the obtained composites. Furthermore, based on the BET analysis results, it was found that the surface area of the composite film was obviously enhanced compared with the synthesized graphene oxide. Electrochemical measurements indicated that the modification of the composites on electrode could efficiently enhance the voltammetric response, suggesting the potential application for making electrochemical sensors.

Synthesis of polyaniline/SnO2 nanocomposite and its improved electrochemical performance

International Nuclear Information System (INIS)

Luo, Zhenyu; Zhu, Yinhai; Liu, Enhui; Hu, Tiantian; Li, Zengpeng; Liu, Tiantian; Song, Longchu

2014-01-01

Highlights: • Supercapacitors based on PANI/SnO 2 nanocomposite were reported. • Supercapacitors using this material gave a specific capacitance of 501 F g −1 . • Capacitance retention was 85.8% over 2000 charge–discharge cycles. - Abstract: SnO 2 was prepared by the hydrothermal route. Aniline monomer was polymerized in the suspension of SnO 2 to form inorganic–organic nanocomposite materials, in which SnO 2 particles were embedded within polyaniline (PANI). Morphological and structural characterizations of the prepared samples were carried out using scanning electron microscope; transmission electron microscope; power X-ray diffraction and Fourier transform infrared spectroscopy. Their electrochemical properties were also investigated using cyclic voltammetry, galvanostatic charge–discharge and electrochemical impedance spectroscopy. The as-prepared nanocomposites had excellent properties in the capacitance, and its specific capacitance was up to 501 F g −1 with a specific energy density of 66.8 W h kg −1 at a power density of 960.6 W kg −1 . The device fulfilled the requirement of long durability necessary for an energy storage system, since after 2000 galvanostatic charge–discharge cycles, retention of 85.8% in capacitance was observed. These results indicated that the PANI/SnO 2 had a synergistic effect of the complementary properties of both components

Electrochemical synthesis of hydrogen peroxide: Rotating disk electrode and fuel cell studies

International Nuclear Information System (INIS)

Lobyntseva, Elena; Kallio, Tanja; Alexeyeva, Nadezda; Tammeveski, Kaido; Kontturi, Kyoesti

2007-01-01

The electrochemical reduction of oxygen on various catalysts was studied using the thin-layer rotating disk electrode (RDE) method. High-surface-area carbon was modified with an anthraquinone derivative and gold nanoparticles. Polytetrafluoroethylene (PTFE) and cationic polyelectrolyte (FAA) were used as binders in the preparation of thin-film electrodes. Our primary goal was to find a good electrocatalyst for the two-electron reduction of oxygen to hydrogen peroxide. All electrochemical measurements were carried out in 0.1 M KOH. Cyclic voltammetry was used in order to characterise the surface processes of the modified electrodes in O 2 -free electrolyte. The RDE results revealed that the carbon-supported gold nanoparticles are active catalysts for the four-electron reduction of oxygen in alkaline solution. Anthraquinone-modified high-area carbon catalyses the two-electron reduction at low overpotentials, which is advantageous for hydrogen peroxide production. In addition, the polymer electrolyte fuel cell technology was used for the generation of hydrogen peroxide. The cell was equipped with a bipolar membrane which consisted of commercial Nafion 117 as a cation-exchange layer and FT-FAA as an anion-exchange layer. The bipolar membranes were prepared by a hot pressing method. Use of the FAA ionomer as a binder for the anthraquinone-modified carbon catalyst resulted in production of hydrogen peroxide

Influence of particle size and fluorination ratio of CFx precursor compounds on the electrochemical performance of C–FeF2 nanocomposites for reversible lithium storage

Directory of Open Access Journals (Sweden)

Ben Breitung

2013-11-01

Full Text Available Systematical studies of the electrochemical performance of CFx-derived carbon–FeF2 nanocomposites for reversible lithium storage are presented. The conversion cathode materials were synthesized by a simple one-pot synthesis, which enables a reactive intercalation of nanoscale Fe particles in a CFx matrix, and the reaction of these components to an electrically conductive C–FeF2 compound. The pretreatment and the structure of the utilized CFx precursors play a crucial role in the synthesis and influence the electrochemical behavior of the conversion cathode material. The particle size of the CFx precursor particles was varied by ball milling as well as by choosing different C/F ratios. The investigations led to optimized C–FeF2 conversion cathode materials that showed specific capacities of 436 mAh/g at 40 °C after 25 cycles. The composites were characterized by Raman spectroscopy, X-Ray diffraction measurements, electron energy loss spectroscopy and TEM measurements. The electrochemical performances of the materials were tested by galvanostatic measurements.

Facile synthesis of Co3O4 nanowires grown on hollow NiO microspheres with superior electrochemical performance

International Nuclear Information System (INIS)

Fan, Meiqing; Ren, Bo; Yu, Lei; Song, Dalei; Liu, Qi; Liu, Jingyuan; Wang, Jun; Jing, Xiaoyan; Liu, Lianhe

2015-01-01

Graphical abstract: Display Omitted - Highlights: • The NiO hollow spheres were decorated by Co 3 O 4 nanowires. • The NiO hollow spheres were comprised of many NiO particles. • The Co 3 O 4 nanowires were composed of nanoparticles. • The NiO/Co 3 O 4 core/shell nanocomposites have good electrochemical properties. - Abstract: The NiO/Co 3 O 4 core/shell composites as a promising supercapacitor material have been fabricated by facile hydrothermal process. The structure and morphology of the NiO/Co 3 O 4 core/shell composites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results indicated that the NiO hollow spheres were decorated by Co 3 O 4 nanowires, and the nanowires were composed of nanoparticles. Electrochemical properties were characterized by cyclic voltammetry, galvanostatic charge/discharge measurements, and electrochemical impedance spectroscopy. The results suggested that the NiO/Co 3 O 4 core/shell composites had good electrochemical reversibility and displayed superior capacitive performance with large capacitance (510 F g −1 ). Moreover, NiO/Co 3 O 4 core/shell composites showed excellent cyclic performanceafter 1000 cycles

Synthesis and electrochemical probing of water-soluble poly(sodium 4-styrenesulfonate-co-acrylic acid)-grafted multiwalled carbon nanotubes

International Nuclear Information System (INIS)

Du Feipeng; Yang Yingkui; Xie Xiaolin; Wu Kangbing; Gan Tian; Liu Lang

2008-01-01

Water-soluble poly(sodium 4-styrenesulfonate-co-acrylic acid)-grafted multiwalled carbon nanotubes (MWNT-g-P(SSS-co-AA)) with core-shell nanostructure were successfully synthesized by in situ free radical copolymerization of sodium 4-strenesulfonate (SSS) and acrylic acid (AA) in the presence of MWNTs terminated with vinyl groups; their structure was characterized by FTIR, 1 H NMR, Raman, TGA and TEM. The results showed that the thickness and content of the copolymer layer grafted onto the MWNT surface are about 7-12 nm and 82.3%, respectively. The P(SSS-co-AA) covalently grafted on MWNTs provides MWNT-g-P(SSS-co-AA) with good hydrophilicity and solubility in water. Then a novel MWNT-g-P(SSS-co-AA)-modified glassy carbon electrode was fabricated by coating; its electrochemical properties were evaluated by electrochemical probe of K 3 [Fe(CN) 6 ], and its catalytic behaviors to the electrochemical oxidation processes of dopamine (DA) and serotonin (5-HT) were investigated. Since the MWNT-g-P(SSS-co-AA)-modified electrode possesses strong electron transfer capability, high electrochemical activity and catalytic ability, it can be used in sensitive, selective, rapid and simultaneous monitoring of biomolecules

Synthesis of Some Novel Pyrimidine Derivatives and Investigation of their Electrochemical Behavior

International Nuclear Information System (INIS)

Akbas, Esvet; Gumus, Selcuk; Sumer, Mehmet Rauf; Akyaz, Inci; Levent, Abdulkadir

2010-01-01

2-Iminopyrimidines (1a-e) and 2-thioxopyrimidine (2) were synthesized using the Biginelli three component cyclocondensation reaction of an appropriate β-diketone, arylaldehyde, and guanidine (for 1a-e) or thiourea (for 2). The electrochemical properties of the novel systems were investigated by CV and DPV. Moreover, B3LYP/6-31G(d,p) method was applied to the present structures in order to gather some structural and physicochemical data

Direct chemical synthesis of MnO2 nanowhiskers on MXene surfaces for supercapacitor applications

KAUST Repository

Baby, Rakhi Raghavan; Ahmed, Bilal; Anjum, Dalaver H.; Alshareef, Husam N.

2016-01-01

Transition metal carbides (MXenes) are an emerging class of two dimensional (2D) materials with promising electrochemical energy storage performance. Herein, for the first time, by direct chemical synthesis, nanocrystalline ε-MnO2 whiskers were

Mixing transition-metal phosphates Li_3V_2_−_xFe_x(PO_4)_3 (0≤x≤2): the synthesis, structure and electrochemical properties

International Nuclear Information System (INIS)

Liu, Xudong; Zhao, Yanming; Kuang, Quan; Li, Xiaoming; Dong, Youzhong; Jing, Zhenzhen; Hou, Shiyu

2016-01-01

Highlights: • Monoclinic structure Li_3V_2_−_xFe_x(PO_4)_3 (0≤ x≤2) solid solutions have been successfully fabricated via a two-step synthesis method. • Trace amounts of acetylene black would play a role of deoxidizer during the sintering process in an inert atmosphere. • V1-site is the preferred position when Fe"3"+ ions doped into Li_3V_2(PO_4)_3 from our structural analysis. - Abstract: Mixing transition-metal phosphates Li_3V_2_−_xFe_x(PO_4)_3 (0≤x≤2) were first designed to be a type of intercalated and deintercalated cathodes to obtain high specific capacity for safe Li-ion batteries. Since the residual oxygen in the quartz tube furnace and pellet would oxidize the V"3"+ to V"4"+ in the Ar ambience during the sintering process, trace amounts of acetylene black inside and outside the pellet could play a role of deoxidizer to protect V"3"+ meanwhile ensure Fe"3"+ not reducing to Fe"2"+. With the concerted effort of inside and outside acetylene black, monoclinic structure Li_3V_2_−_xFe_x(PO_4)_3 (0≤x≤2) solid solutions had been successfully fabricated via a two-step synthesis method. X-ray diffractions with Rietveld refinement revealed that V1-sites were the preferred position when Fe"3"+ ions doped into Li_3V_2(PO_4)_3, which means, every V1-site was occupied with the same probability by V"3"+ and Fe"3"+ when 0< x<1, and then for V2-site when 1< x<2. X-ray photoelectron spectroscopy result showed the presence of trace amounts of acetylene black had realized the coexist of V"3"+ and Fe"3"+ in the Li_3M_2(PO_4)_3 framework. When evaluated as cathodes for Li-ion batteries, the pure Li_3V_2(PO_4)_3 electrode displayed the highest charge (137.2 mAh g"−"1) and discharge (121.5 mAh g"−"1) capacities in the first cycle, with the increase of Fe"3"+ content, all the charge and discharge capacities reduced drastically. Furthermore, the EIS results showed that the incorporation of the sluggish Fe"3"+ ions reduced the electronic conductivity and

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

International Nuclear Information System (INIS)

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

2013-01-01

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

Hybrid nanostructured materials for high-performance electrochemical capacitors

KAUST Repository

Yu, Guihua

2013-03-01

The exciting development of advanced nanostructured materials has driven the rapid growth of research in the field of electrochemical energy storage (EES) systems which are critical to a variety of applications ranging from portable consumer electronics, hybrid electric vehicles, to large industrial scale power and energy management. Owing to their capability to deliver high power performance and extremely long cycle life, electrochemical capacitors (ECs), one of the key EES systems, have attracted increasing attention in the recent years since they can complement or even replace batteries in the energy storage field, especially when high power delivery or uptake is needed. This review article describes the most recent progress in the development of nanostructured electrode materials for EC technology, with a particular focus on hybrid nanostructured materials that combine carbon based materials with pseudocapacitive metal oxides or conducting polymers for achieving high-performance ECs. This review starts with an overview of EES technologies and the comparison between various EES systems, followed by a brief description of energy storage mechanisms for different types of EC materials. This review emphasizes the exciting development of both hybrid nanomaterials and novel support structures for effective electrochemical utilization and high mass loading of active electrode materials, both of which have brought the energy density of ECs closer to that of batteries while still maintaining their characteristic high power density. Last, future research directions and the remaining challenges toward the rational design and synthesis of hybrid nanostructured electrode materials for next-generation ECs are discussed. © 2012 Elsevier Ltd.

Facile synthesis and strongly microstructure-dependent electrochemical properties of graphene/manganese dioxide composites for supercapacitors

Science.gov (United States)

Zhang, Caiyun; Zhu, Xiaohong; Wang, Zhongxing; Sun, Ping; Ren, Yinjuan; Zhu, Jiliang; Zhu, Jianguo; Xiao, Dingquan

2014-09-01

Graphene has attracted much attention since it was firstly stripped from graphite by two physicists in 2004, and the supercapacitor based on graphene has obtained wide attention and much investment as well. For practical applications of graphene-based supercapacitors, however, there are still many challenges to solve, for instance, to simplify the technological process, to lower the fabrication cost, and to improve the electrochemical performance. In this work, graphene/MnO2 composites are prepared by a microwave sintering method, and we report here a relatively simple method for the supercapacitor packaging, i.e., dipping Ni-foam into a graphene/MnO2 composite solution directly for a period of time to coat the active material on a current collector. It is found that the microwave reaction time has a significant effect on the microstructure of graphene/MnO2 composites, and consequently, the electrochemical properties of the supercapacitors based on graphene/MnO2 composites are strongly microstructure dependent. An appropriately longer microwave reaction time, namely, 15 min, facilitates a very dense and homogeneous microstructure of the graphene/MnO2 composites, and thus, excellent electrochemical performance is achieved in the supercapacitor device, including a high specific capacitance of 296 F/g and a high capacitance retention of 93% after 3,000 times of charging/discharging cycles.

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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

International Nuclear Information System (INIS)

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

2013-01-01

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

Synthesis of gold nanoparticles on the surface of pyrolytic graphite using penicillin as a stabilizing reagent and the catalytic oxidation of α-naphthylamine

Science.gov (United States)

Song, Y. Z.; Song, Y.; Cheng, Z. P.; Zhou, J. F.; Wei, C.

2013-01-01

Electrochemical synthesis of gold nanoparticles on the surface of pyrolytic graphite using penicillin as a stabilizing reagent was proposed. The gold nanoparticles were characterized by scanning electron microscopy, cyclic voltammetry, IR spectra, UV spectra, and powder X-ray diffraction spectra. The electro-chemical catalysis of penicillin for α-naphthylamine was demonstrated.

Synthesis of Biokerosene through Electrochemical Hydrogenation of Terpene Hydrocarbons from Turpentine Oil

Directory of Open Access Journals (Sweden)

Tedi Hudaya

2016-12-01

Full Text Available Indonesia possesses great potential for developing renewable resources as alternative fuels. For example, turpentine oil obtained from Pinus merkusii, which contains mostly monoterpene hydrocarbons (C10H16. The oil is highly suitable to be processed for biokerosene or even jet biofuel. It consists of hydrocarbons within the range of C10 to C15. However, it contains insufficient H and thus needs to be upgraded. In the present work, electrochemical hydrogenation was used for upgrading. In the electrochemical cell, stainless steel, silver, and carbon were used alternately for the anode, while copper and silver Raschig rings were used for the cathode. An electrolyte solution of cuprous ammonium formate was utilized not only as a source of H but also to draw the unsaturated hydrocarbons into the aqueous phase. The electrolyte : oil ratio (up to 2:1, electrolyte concentration (between 0.4 and 2 M and reaction time were varied throughout the experiments. The bromine number (unsaturation level of the turpentine oil, which was initially 1,86 (mole Br2/mole, was lowered significantly to 0.69-0.90. Promising increase of smoke point values were observed from 11 mm to 16-24 mm, indicating a higher H content of the processed oil, thus making it suitable as a substitute for petroleum kerosene.

A one-pot chemoselective synthesis of secondary amines by using a biomimetic electrocatalytic system

International Nuclear Information System (INIS)

Largeron, Martine

2009-01-01

A one-pot electrochemically induced oxidation-imine formation-reduction route to secondary amines is described in detail. The key step of the process consists of the o-iminoquinone-mediated chemoselective catalytic oxidation of a primary aliphatic amine substrate, in the presence of a second amine used as the alkylating agent. Through the examination of the scope of the reaction by systematically varying both amine substrate and amine alkylating agent, it can be shown that this reaction sequence, leaving ammonia as the sole by-product, allows the rapid synthesis of various secondary amines in moderate to good yields. This process, that highlights the pre-eminent green advantages of electrochemical synthesis, especially the utilization of electricity as energy instead of chemical reagents, high atom economy as well as ambient temperature and pressure, could be a mild alternative to already reported synthetic methods.

A one-pot chemoselective synthesis of secondary amines by using a biomimetic electrocatalytic system

Energy Technology Data Exchange (ETDEWEB)

Largeron, Martine [UMR CNRS 8638, Synthese et Structure de Molecules d' nteret Pharmacologique, Universite Paris Descartes, Faculte des Sciences Pharmaceutiques et Biologiques, 4 Avenue de l' Observatoire, 75270 Paris Cedex 06 (France)], E-mail: martine.largeron@parisdescartes.fr

2009-09-01

A one-pot electrochemically induced oxidation-imine formation-reduction route to secondary amines is described in detail. The key step of the process consists of the o-iminoquinone-mediated chemoselective catalytic oxidation of a primary aliphatic amine substrate, in the presence of a second amine used as the alkylating agent. Through the examination of the scope of the reaction by systematically varying both amine substrate and amine alkylating agent, it can be shown that this reaction sequence, leaving ammonia as the sole by-product, allows the rapid synthesis of various secondary amines in moderate to good yields. This process, that highlights the pre-eminent green advantages of electrochemical synthesis, especially the utilization of electricity as energy instead of chemical reagents, high atom economy as well as ambient temperature and pressure, could be a mild alternative to already reported synthetic methods.

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

Science.gov (United States)

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

Organic-inorganic hybrid polymer electrolytes based on polyether diamine, alkoxysilane, and trichlorotriazine: Synthesis, characterization, and electrochemical applications

Science.gov (United States)

Saikia, Diganta; Wu, Cheng-Gang; Fang, Jason; Tsai, Li-Duan; Kao, Hsien-Ming

2014-12-01

A new type of highly conductive organic-inorganic hybrid polymer electrolytes has been synthesized by the reaction of poly(propylene glycol)-block-poly(ethylene glycol)-block-poly(propylene glycol) bis(2-aminopropyl ether), 2,4,6-trichloro-1,3,5-triazine and alkoxysilane precursor 3-(glycidyloxypropyl)trimethoxysilane, followed by doping of LiClO4. The 13C and 29Si solid-sate NMR results confirm the successful synthesis of the organic-inorganic hybrid structure. The solid hybrid electrolyte thus obtained exhibits a maximum ionic conductivity of 1.6 × 10-4 S cm-1 at 30 °C, which is the highest among the organic-inorganic hybrid electrolytes. The hybrid electrolytes are electrochemically stable up to 4.2 V. The prototype electrochromic device with such a solid hybrid electrolyte demonstrates a good coloration efficiency value of 183 cm2 C-1 with a cycle life over 200 cycles. For the lithium-ion battery test, the salt free solid hybrid membrane is swelled with a LiPF6-containing electrolyte solution to reach an acceptable ionic conductivity value of 6.5 × 10-3 S cm-1 at 30 °C. The battery cell carries an initial discharge capacity of 100 mAh g-1 at 0.2C-rate and a coulombic efficiency of about 95% up to 30 cycles without the sign of cell failure. The present organic-inorganic hybrid electrolytes hold promise for applications in electrochromic devices and lithium ion batteries.

Utilization of plasmas for graphene synthesis

Science.gov (United States)

Shashurin, Alexey; Keidar, Michael

2013-10-01

Graphene is a one-atom-thick planar sheet of carbon atoms that are densely packed in a honeycomb crystal lattice. Grapheen has tremendous range of potential applications ranging from high-speed transistors to electrochemical energy storage devices and biochemical sensors. Methods of graphene synthesis include mechanical exfoliation, epitaxial growth on SiC, CVD and colloidal suspensions. In this work the utilization of plasmas in synthesis process is considered. Types of carbonaceous structures produced by the anodic arc and regions of their synthesis were studied. Ultimate role of substrate temperature and transformations occurring with various carbonaceous structures generated in plasma discharge were considered. Formation of graphene film on copper substrate was detected at temperatures around the copper melting point. The film was consisted of several layers graphene flakes having typical sizes of about 200 nm. Time required for crystallization of graphene on externally heated substrates was determined. This work was supported by National Science Foundation (NSF Grant No. CBET-1249213).

Synthesis, characterization and electrochemical investigations of mixed-ligand copper(II)-organic supramolecular frameworks

Science.gov (United States)

Singh, Sandeep K.; Srivastava, Ashish Kumar; Srivastava, Krishna; Banerjee, Rahul; Prasad, Jagdish

2017-11-01

Two mixed-ligand copper(II)-organic coordination compounds with 5,5‧-dimethyl-2,2‧-bipyridine (5,5‧-Me2bpy) as a primary ligand while aliphatic malonate (Hmal) and aromatic 2-hydroxynicotinate (2-OHNA) as secondary ligands, were synthesized. These complexes are formulated as: [Cu(Hmal)(5,5‧-Me2bpy)(H2O)](ClO4) 1 and [Cu2(2-OHNA)2(5,5‧-Me2bpy)2(NO3)](NO3) 2. These two complexes were structurally characterized by single crystal X-ray diffraction analysis. Characterization was further supported by powder X-ray diffraction analysis, elemental analyses, FT-IR, FAB-MASS and TGA, DSC studies. Cyclic voltammetric and UV-visible spectral studies of these two complexes have also been done. The electrochemical studies of complex 1 in DMSO and DMF have shown that this complex undergoes quasi-reversible diffusion-controlled one-electron transfer reaction without any chemical complication while complex 2 in DMSO undergoes quasi-reversible diffusion-controlled one electron transfer reaction, following EC mechanism. The electrochemical behaviour of complex 2 in DMF is complicated probably due to presence of more than one species in solution phase.

Calix[6]arene mono-diazonium salt synthesis and covalent immobilization onto glassy carbon electrodes

International Nuclear Information System (INIS)

Cannizzo, Caroline; Jasmin, Jean-Philippe; Vautrin-Ul, Christine; Chausse, Annie; Wagner, Mathieu; Doizi, Denis; Lamouroux, Christine

2014-01-01

This Letter describes the fast synthesis of a mono-aminated calix[6]arene. The immobilization of this macrocycle onto glassy carbon electrodes via diazonium salt chemistry and the electrochemical characterization of the grafted organic layer are also reported. (authors)

Conducting polymers: Synthesis and industrial applications

Energy Technology Data Exchange (ETDEWEB)

Gottesfeld, S. [Los Alamos National Laboratory, NM (United States)

1995-05-01

The Conducting Polymer project funded by the AIM Materials Program is developing new methods for the synthesis of electronically conducting polymers and is evaluating new industrial applications for these materials which will result in significant reductions in energy usage or industrial waste. The applications specifically addressed during FY 1994 are electrochemical capacitors and membranes for gas separation. As an active material in electrochemical capacitors, conducting polymers have the potential of storing large amounts of electrical energy in low cost materials. Such devices are needed in electronics for power failure back-up and peak power, in power supplies for filtering, and in electric vehicles for peak power and load leveling. As a gas electrically adapt the membrane for specific gas combinations. Potential energy savings in the US. for this application are estimated at 1 to 3 quads/yr.

Effects of synthetic parameters on structure and electrochemical performance of spinel lithium manganese oxide by citric acid-assisted sol-gel method

International Nuclear Information System (INIS)

Yi Tingfeng; Dai Changsong; Gao Kun; Hu Xinguo

2006-01-01

The spinel lithium manganese oxide cathode materials were prepared by citric acid-assisted sol-gel method at 623-1073 K in air. The effects of pH value, raw material, synthesis temperature and time on structure and electrochemical performance of spinel lithium manganese oxide are investigated by X-ray diffraction (XRD), scanning electronic microscope (SEM) and cyclic voltammetry (CV). XRD data results strongly suggest that the synthesis temperature is the dominating factors of the formation of spinel phase, and spinel lithium manganese oxide powder with various crystallites size can be obtained by controlling the sintering time. CV shows that spinel lithium manganese oxide powder formed about 973 K presents the best electrochemical performance with well separated two peaks and the highest peak current. Charge-discharge test indicates that spinel lithium manganese oxide powders calcined at higher temperatures have high discharge capacity and capacity loss, and sintered at lower temperatures has low discharge capacity and high capacity retention

Effects of synthetic parameters on structure and electrochemical performance of spinel lithium manganese oxide by citric acid-assisted sol-gel method

Energy Technology Data Exchange (ETDEWEB)

Yi Tingfeng [Department of Applied Chemistry, Harbin Institute of Technology, Harbin 150001 (China)]. E-mail: tfyihit@hit.edu.cn; Dai Changsong [Department of Applied Chemistry, Harbin Institute of Technology, Harbin 150001 (China); Gao Kun [Department of Applied Chemistry, Harbin Institute of Technology, Harbin 150001 (China); Hu Xinguo [Department of Applied Chemistry, Harbin Institute of Technology, Harbin 150001 (China)

2006-11-30

The spinel lithium manganese oxide cathode materials were prepared by citric acid-assisted sol-gel method at 623-1073 K in air. The effects of pH value, raw material, synthesis temperature and time on structure and electrochemical performance of spinel lithium manganese oxide are investigated by X-ray diffraction (XRD), scanning electronic microscope (SEM) and cyclic voltammetry (CV). XRD data results strongly suggest that the synthesis temperature is the dominating factors of the formation of spinel phase, and spinel lithium manganese oxide powder with various crystallites size can be obtained by controlling the sintering time. CV shows that spinel lithium manganese oxide powder formed about 973 K presents the best electrochemical performance with well separated two peaks and the highest peak current. Charge-discharge test indicates that spinel lithium manganese oxide powders calcined at higher temperatures have high discharge capacity and capacity loss, and sintered at lower temperatures has low discharge capacity and high capacity retention.

An Electrochemical pH Sensor Based on the Amino-Functionalized Graphene and Polyaniline Composite Film.

Science.gov (United States)

Su, W; Xu, J; Ding, Xianting

2016-12-01

Conventional glass-based pH sensors are usually fragile and space consuming. Herein, a miniature electrochemical pH sensor based on amino-functionalized graphene fragments and polyaniline (NH 2 -G/PANI) composite film is developed via simply one-pot electrochemical polymerization on the ITO-coated glass substrates. Cyclic Voltammetry (CV), Scanning Electron Microscopy (SEM), Transmission electron microscopy (TEM), X-ray Photoelectron Spectroscopy (XPS), and Raman Spectra are involved to confirm the successful synthesis and to characterize the properties of the NH 2 -G/PANI composite film. The developed electrochemical pH sensor presents fast response, high sensitivity (51.1 mV/pH) and wide detection range when applied to PBS solutions of pH values from 1 to 11. The robust reproducibility and good stability of the developed pH sensors are investigated as well. Compared to the conventional glass-based pH meters, the NH 2 -G/PANI composite film-based pH sensor could be a promising contender for the flexible and miniaturized pH-sensing devices.

Electrochemical Oxidation of Propene with a LSF15/CGO10 Electrochemical Reactor

DEFF Research Database (Denmark)

Ippolito, Davide; Kammer Hansen, Kent

2014-01-01

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

Facile synthesis of Co(OH)2/Al(OH)3 nanosheets with improved electrochemical properties for asymmetric supercapacitor

Science.gov (United States)

Zhao, Cuimei; Ren, Fang; Cao, Yang; Xue, Xiangxin; Duan, Xiaoyue; Wang, Hairui; Chang, Limin

2018-01-01

Sheet-like Co(OH)2/Al(OH)3 or Co(OH)2 nanomaterial has been synthesized on conducting carbon fiber paper (CFP) by a facile one-step electrochemical deposition. The binder-free Co(OH)2/Al(OH)3/CFP displays an improved electrical conductivity, electrochemical activity and material utilization than solitary Co(OH)2, therefore Co(OH)2/Al(OH)3 nanomaterial exhibits improved electrochemical properties (a maximum capacitance of 1006 Fg-1 at 2 Ag-1, with 77% retention even at a high current density of 32 Ag-1, and more than 87% of the capacitance retention after 10000 cycles at 32 Ag-1) in comparison to that of the Co(OH)2/CFP (709 Fg-1, 65%, 79%). In addition, an asymmetric supercapacitor (ASC) fabricated with Co(OH)2/Al(OH)3/CFP positive electrode and AC/CFP negative electrode demonstrates ultrahigh specific capacitance (75.8 Fg-1) and potential window (1.7 V). These encouraging results make these low-cost and eco-friendly materials promising for high-performance energy storage application.

Fast and low-cost synthesis of 1D ZnO–TiO{sub 2} core–shell nanoarrays: Characterization and enhanced photo-electrochemical performance for water splitting

Energy Technology Data Exchange (ETDEWEB)

Hernández, Simelys, E-mail: simelys.hernandez@iit.it [Center for Space Human Robotics (IIT-POLITO), Istituto Italiano di Tecnologia, Corso Trento 21, 10129 Torino (Italy); Cauda, Valentina; Hidalgo, Diana; Farías Rivera, Vivian; Manfredi, Diego; Chiodoni, Angelica [Center for Space Human Robotics (IIT-POLITO), Istituto Italiano di Tecnologia, Corso Trento 21, 10129 Torino (Italy); Pirri, Fabrizio C. [Center for Space Human Robotics (IIT-POLITO), Istituto Italiano di Tecnologia, Corso Trento 21, 10129 Torino (Italy); Applied Science and Technology Department, Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino (Italy)

2014-12-05

Highlights: • Simple, fast and low-cost synthesis of 1-D ZnO–TiO{sub 2} core–shell heterostructures. • ZnO NWs completely covered with a shell of anatase TiO{sub 2} nanocrystals in only 3 min. • The TiO{sub 2} shell thickness depends on the impregnation time in the titania synthesis bath. • 2-fold enhancement of photo-electrochemical activity and better stability of ZnONWs. • Forty- times higher photocurrent densities than TiO{sub 2} nanoparticles film. - Abstract: We report on a simple, fast and low-cost synthesis procedure for the complete covering of zinc oxide (ZnO) 1D nanostructures with a protective shell of titania (TiO{sub 2}) nanoparticles. ZnO nanowires (NWs) were grown on transparent F-doped Tin Oxide (FTO) conductive layer on glass by seed layer-assisted hydrothermal route in aqueous media, while the titania shell was deposited on the ZnO NWs through an in situ non-acid sol–gel synthesis. The nanowires impregnation time in the titania sol was varied from 3 to 10 min. The resulting core–shell ZnO–TiO{sub 2} structures were characterized by different techniques, including Scanning and Transmission Electron Microscopy, X-ray diffraction and UV–Vis spectroscopy, confirming the uniform coverage of the wurzite ZnO NWs with anatase TiO{sub 2} nanoparticles (NPs), with a shell thickness dependent on the impregnation time in the titania synthesis bath. Photoelectrochemical (PEC) tests of the ZnO–TiO{sub 2} material, used as anode for the water splitting reaction, confirmed the formation of the heterojunction by the enhanced photocurrent densities, reaching values of about 0.7 mA/cm{sup 2} under simulated solar light (AM1.5G, 100mW/cm{sup 2}). The core–shell photo-anodes performance was about twice and forty- times better than the ones with a film of equivalent thickness of bare ZnO NWs and TiO{sub 2} NPs, respectively. Steady-state measures of the photocurrent over the time and FESEM analysis confirmed that this procedure could be

Synthesis, spectroscopic analysis and electrochemical performance of modified β-nickel hydroxide electrode with CuO

Directory of Open Access Journals (Sweden)

B. Shruthi

2017-03-01

Full Text Available In the present work, a modified β-nickel hydroxide (β-Ni(OH2 electrode material with CuO has been prepared using a co-precipitation method. The structure and property of the modified β-Ni(OH2 with CuO were characterized by X-ray diffraction (XRD, Fourier Transform infra-red (FT-IR, Raman and thermal gravimetric-differential thermal analysis (TG-DTA techniques. The results of the FT-IR spectroscopy and TG-DTA indicate that the modified β-Ni(OH2 electrode materials contain intercalated water molecules and anions. A pasted–type electrode was prepared using nickel hydroxide powder as the main active material on a nickel sheet as a current collector. Cyclic voltammetry (CV and Electrochemical impedance spectroscopy (EIS studies were undertaken to assess the electrochemical behavior of pure β-Ni(OH2 and modified β-Ni(OH2 electrode with CuO in a 6 M KOH electrolyte. The addition of CuO into β-nickel hydroxide was found to enhance the reversibility of the electrode reaction and also increase the separation of the oxidation current peak of the active material from the oxygen evolution current. The modified nickel hydroxide with CuO was also found to exhibit a higher proton diffusion coefficient and a lower charge transfer resistance. These findings suggest that the modified β-Ni(OH2 with CuO possesses an enhanced electrochemical response and thus can be recognized as a promising candidate for battery electrode applications.

Facile synthesis and strongly microstructure-dependent electrochemical properties of graphene/manganese dioxide composites for supercapacitors

Science.gov (United States)

2014-01-01

Graphene has attracted much attention since it was firstly stripped from graphite by two physicists in 2004, and the supercapacitor based on graphene has obtained wide attention and much investment as well. For practical applications of graphene-based supercapacitors, however, there are still many challenges to solve, for instance, to simplify the technological process, to lower the fabrication cost, and to improve the electrochemical performance. In this work, graphene/MnO2 composites are prepared by a microwave sintering method, and we report here a relatively simple method for the supercapacitor packaging, i.e., dipping Ni-foam into a graphene/MnO2 composite solution directly for a period of time to coat the active material on a current collector. It is found that the microwave reaction time has a significant effect on the microstructure of graphene/MnO2 composites, and consequently, the electrochemical properties of the supercapacitors based on graphene/MnO2 composites are strongly microstructure dependent. An appropriately longer microwave reaction time, namely, 15 min, facilitates a very dense and homogeneous microstructure of the graphene/MnO2 composites, and thus, excellent electrochemical performance is achieved in the supercapacitor device, including a high specific capacitance of 296 F/g and a high capacitance retention of 93% after 3,000 times of charging/discharging cycles. PACS 81.05.ue; 78.67.Sc; 88.80.fh PMID:25258609

Cathode materials produced by spray flame synthesis for lithium ion batteries

Energy Technology Data Exchange (ETDEWEB)

Hamid, NoorAshrina Binti A.

2013-07-03

Lithium ion batteries are one of the most enthralling rechargeable energy storage systems for portable application due to their high energy density. Nevertheless, with respect to electromobility innovation towards better electrochemical properties such as higher energy and power density is required. Altering the cathode material used in Li-ion batteries is favorable since the mass- and volume performance is closely related to the cathode electrode mass. Instead of using LiCoO{sub 2} as cathode electrode, LiFePO{sub 4} has gained serious attention as this material owns a high theoretical capacity of 170 mAh g{sup -1}. It is non-toxic, cheap and consists of abundant materials but suffers from low electronic and ionic conductivity. Utilization of nanotechnology methods in combination with composite formation is known to cure this problem effectively. In this work, a new combination of techniques using highly scalable gas-phase synthesis namely spray-flame synthesis and subsequent solid-state reaction has been used to synthesize nanocomposite LiFePO{sub 4}/C. At first this work deals with the formation and characterization of nanosize FePO{sub 4} from a solution of iron(III)acetylacetonate and tributyl phosphate in toluene using spray-flame synthesis. It was shown that a subsequent solid state reaction with Li{sub 2}CO{sub 3} and glucose yielded a LiFePO{sub 4}/C nanocomposite with very promising electrochemical properties. Based on these initial findings the influence of two synthesis parameter - carbon content and annealing temperature - was investigated towards the physicochemical properties of LiFePO{sub 4}/C. It was shown that an annealing temperature of 700 C leads to high purity composite materials consisting of crystalline LiFePO{sub 4} with crystallite sizes well below 100 nm and amorphous carbon consisting of disordered and graphite-like carbon. Variation of glucose amount between 10 and 30 wt% resulted in carbon contents between 2.1 and 7.3 wt%. In parallel

Cathode materials produced by spray flame synthesis for lithium ion batteries

Energy Technology Data Exchange (ETDEWEB)

Hamid, NoorAshrina Binti A.

2013-07-03

Lithium ion batteries are one of the most enthralling rechargeable energy storage systems for portable application due to their high energy density. Nevertheless, with respect to electromobility innovation towards better electrochemical properties such as higher energy and power density is required. Altering the cathode material used in Li-ion batteries is favorable since the mass- and volume performance is closely related to the cathode electrode mass. Instead of using LiCoO{sub 2} as cathode electrode, LiFePO{sub 4} has gained serious attention as this material owns a high theoretical capacity of 170 mAh g{sup -1}. It is non-toxic, cheap and consists of abundant materials but suffers from low electronic and ionic conductivity. Utilization of nanotechnology methods in combination with composite formation is known to cure this problem effectively. In this work, a new combination of techniques using highly scalable gas-phase synthesis namely spray-flame synthesis and subsequent solid-state reaction has been used to synthesize nanocomposite LiFePO{sub 4}/C. At first this work deals with the formation and characterization of nanosize FePO{sub 4} from a solution of iron(III)acetylacetonate and tributyl phosphate in toluene using spray-flame synthesis. It was shown that a subsequent solid state reaction with Li{sub 2}CO{sub 3} and glucose yielded a LiFePO{sub 4}/C nanocomposite with very promising electrochemical properties. Based on these initial findings the influence of two synthesis parameter - carbon content and annealing temperature - was investigated towards the physicochemical properties of LiFePO{sub 4}/C. It was shown that an annealing temperature of 700 C leads to high purity composite materials consisting of crystalline LiFePO{sub 4} with crystallite sizes well below 100 nm and amorphous carbon consisting of disordered and graphite-like carbon. Variation of glucose amount between 10 and 30 wt% resulted in carbon contents between 2.1 and 7.3 wt%. In parallel

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

Science.gov (United States)

2018-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-02-28

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

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

International Nuclear Information System (INIS)

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

2017-01-01

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

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

Science.gov (United States)

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.

Synthesis and photophysical characterizations of thermal-stable naphthalene benzimidazoles.

Science.gov (United States)

Erten-Ela, Sule; Ozcelik, Serdar; Eren, Esin

2011-07-01

Microwave-assisted synthesis, photophysical and electrochemical properties of thermal-stable naphthalene benzimidazoles and naphthalimides are studied in this paper. Microwave-assisted synthesis of naphthalene benzimidazoles provide higher yields than the conventional thermal synthesis. Comparative photophysical properties of naphthalene benzimidazoles and naphthalimides are revealed that conjugation of electron-donating group onto naphthalimide moiety increases fluorescence quantum yields. Fluorophore-solvent interactions are also investigated using Lippert-Mataga equation for naphthalimides and naphthalene benzimidazoles. Thermal stabilities of naphthalene benzimidazoles are better than naphthalimides due to increased aromaticity. The experimental E(LUMO) levels of naphthalene benzimidazoles are found to be between 3.15 and 3.28 eV. Therefore, naphthalene benzimidazole derivatives consisting of anchoring groups are promising materials in organic dye sensitized solar cells. © Springer Science+Business Media, LLC 2011

Electrochemical Water Oxidation by a Catalyst-Modified Metal-Organic Framework Thin Film

Energy Technology Data Exchange (ETDEWEB)

Lin, Shaoyang; Pineda-Galvan, Yuliana; Maza, William A.; Epley, Charity C.; Zhu, Jie; Kessinger, Matthew C.; Pushkar, Yulia; Morris, Amanda J. (VP); (Purdue)

2016-12-15

Water oxidation, a key component in artificial photosynthesis, requires high overpotentials and exhibits slow reaction kinetics that necessitates the use of stable and efficient heterogeneous water-oxidation catalysts (WOCs). Here, we report the synthesis of UiO-67 metal–organic framework (MOF) thin films doped with [Ru(tpy)(dcbpy)OH2]2+ (tpy=2,2':6',2''-terpyridine, dcbpy=5,5'-dicarboxy-2,2'-bipyridine) on conducting surfaces and their propensity for electrochemical water oxidation. The electrocatalyst oxidized water with a turnover frequency (TOF) of (0.2±0.1) s-1 at 1.71 V versus the normal hydrogen electrode (NHE) in buffered solution (pH~7) and exhibited structural and electrochemical stability. The electroactive sites were distributed throughout the MOF thin film on the basis of scan-ratedependent voltammetry studies. This work demonstrates a promising way to immobilize large concentrations of electroactive WOCs into a highly robust MOF scaffold and paves the way for future photoelectrochemical water-splitting systems.

Hierarchical architecture of ReS{sub 2}/rGO composites with enhanced electrochemical properties for lithium-ion batteries

Energy Technology Data Exchange (ETDEWEB)

Qi, Fei; Chen, Yuanfu, E-mail: yfchen@uestc.edu.cn; Zheng, Binjie; He, Jiarui; Li, Qian; Wang, Xinqiang; Lin, Jie; Zhou, Jinhao; Yu, Bo; Li, Pingjian; Zhang, Wanli

2017-08-15

Highlights: • The ReS{sub 2}/rGO composites have been synthesized by a facile one-pot method. • The ReS{sub 2}/rGO composites exhibit hierarchical architecture. • The ReS{sub 2}/rGO composites deliver better electrochemical performances than ReS{sub 2}. • The enhanced performance is due to porous and conductive structure of ReS{sub 2}/rGO. - Abstract: Rhenium disulfide (ReS{sub 2}), a two-dimensional (2D) semiconductor, has attracted more and more attention due to its unique anisotropic electronic, optical, mechanical properties. However, the facile synthesis and electrochemical property of ReS{sub 2} and its composite are still necessary to be researched. In this study, for the first time, the ReS{sub 2}/reduced graphene oxide (rGO) composites have been synthesized through a facile and one-pot hydrothermal method. The ReS{sub 2}/rGO composites exhibit a hierarchical, interconnected, and porous architecture constructed by nanosheets. As anode for lithium-ion batteries, the as-synthesized ReS{sub 2}/rGO composites deliver a large initial capacity of 918 mAh g{sup −1} at 0.2 C. In addition, the ReS{sub 2}/rGO composites exhibit much better electrochemical cycling stability and rate capability than that of bare ReS{sub 2}. The significant enhancement in electrochemical property can be attributed to its unique architecture constructed by nanosheets and porous structure, which can allow for easy electrolyte infiltration, efficient electron transfer, and ionic diffusion. Furthermore, the graphene with high electronic conductivity can provide good conductive passageways. The facile synthesis approach can be extended to prepare other 2D transition metal dichalcogenides semiconductors for energy storage and catalytic application.

Electrochemical Synthesis of Polypyrrole, Reduced Graphene Oxide, and Gold Nanoparticles Composite and Its Application to Hydrogen Peroxide Biosensor

Directory of Open Access Journals (Sweden)

Baoyan Wu

2016-11-01

Full Text Available Here we report a facile eco-friendly one-step electrochemical approach for the fabrication of a polypyrrole (PPy, reduced graphene oxide (RGO, and gold nanoparticles (nanoAu biocomposite on a glassy carbon electrode (GCE. The electrochemical behaviors of PPy–RGO–nanoAu and its application to electrochemical detection of hydrogen peroxide were investigated by cyclic voltammetry. Graphene oxide and pyrrole monomer were first mixed and casted on the surface of a cleaned GCE. After an electrochemical processing consisting of the electrooxidation of pyrrole monomer and simultaneous electroreduction of graphene oxide and auric ions (Au3+ in aqueous solution, a PPy–RGO–nanoAu biocomposite was synthesized on GCE. Each component of PPy–RGO–nanoAu is electroactive without non-electroactive substance. The obtained PPy–RGO–nanoAu/GCE exhibited high electrocatalytic activity toward hydrogen peroxide, which allows the detection of hydrogen peroxide at a negative potential of about −0.62 V vs. SCE. The amperometric responses of the biosensor displayed a sensitivity of 40 µA/mM, a linear range of 32 µM–2 mM, and a detection limit of 2.7 µM (signal-to-noise ratio = 3 with good stability and acceptable reproducibility and selectivity. The results clearly demonstrate the potential of the as-prepared PPy–RGO–nanoAu biocomposite for use as a highly electroactive matrix for an amperometric biosensor.

Sol-Gel Synthesis, Electrochemical Characterization, and Stability Testing of Ti0.7W0.3O2 Nanoparticles for Catalyst Support Applications in Proton-Exchange Membrane Fuel Cells

Energy Technology Data Exchange (ETDEWEB)

Subban, Chinmayee V. [Cornell Univ., Ithaca, NY (United States); Zhou, Qin [Cornell Univ., Ithaca, NY (United States); Hu, Anthony [Cornell Univ., Ithaca, NY (United States); Moylan, Thomas E. [General Motors Research and Development, Warren, MI (United States); Wagner, Frederick T. [General Motors Research and Development, Warren, MI (United States); DiSalvo, Francis J. [Cornell Univ., Ithaca, NY (United States)

2010-11-19

The materials currently used in proton-exchange membrane fuel cells (PEMFCs) require complex control of operating conditions to make them sufficiently durable to permit commercial deployment. One of the major materials challenges to allow simplification of fuel cell operating strategies is the discovery of catalyst supports that are much more stable to oxidative decomposition than currently used carbon blacks. Here we report the synthesis and characterization of Ti_0.7W_0.3O₂ nanoparticles (approximately 50 nm diameter), a promising doped metal oxide that is a candidate for such a durable catalyst support. The synthesized nanoparticles were platinized, characterized by electrochemical testing, and evaluated for stability under PEMFC and other oxidizing acidic conditions. Ti_0.7W_0.3O₂ nanoparticles show no evidence of decomposition when heated in a Nafion solution for 3 weeks at 80 °C. In contrast, when heated in sulfuric, nitric, perchloric, or hydrochloric acid, the oxide reacts to form salts such as titanylsulfatehydrate from sulfuric acid. Electrochemical tests show that rates of hydrogen oxidation and oxygen reduction by platinum nanoparticles supported on Ti_0.7W_0.3O₂ are comparable to those of commercial Pt on carbon black.

Electrochemical study of lithium insertion into carbon-rich polymer-derived silicon carbonitride ceramics

International Nuclear Information System (INIS)

Kaspar, Jan; Mera, Gabriela; Nowak, Andrzej P.; Graczyk-Zajac, Magdalena; Riedel, Ralf

2010-01-01

This paper presents the lithium insertion into carbon-rich polymer-derived silicon carbonitride (SiCN) ceramic synthesized by the thermal treatment of poly(diphenylsilylcarbodiimide) at three temperatures, namely 1100, 1300, and 1700 o C under 0.1 MPa Ar atmosphere. At lower synthesis temperatures, the material is X-ray amorphous, while at 1700 o C, the SiCN ceramic partially crystallizes. Anode materials prepared from these carbon-rich SiCN ceramics without any fillers and conducting additives were characterized using cyclic voltammetry and chronopotentiometric charging/discharging. We found that the studied silicon carbonitride ceramics demonstrate a promising electrochemical behavior during lithium insertion/extraction in terms of capacity and cycling stability. The sample synthesized at 1300 o C exhibits a reversible capacity of 392 mAh g -1 . Our study confirms that carbon-rich SiCN phases are electrochemically active materials in terms of Li inter- and deintercalation.

Ammonia synthesis from N2 and H2O using a lithium cycling electrification strategy at atmospheric pressure

DEFF Research Database (Denmark)

McEnaney, Joshua M.; Singh, Aayush R.; Schwalbe, Jay A.

2017-01-01

Ammonia production is imperative to providing food for a growing world population. However, the primary method of synthetic ammonia production, the Haber Bosch process, is resource demanding and unsustainable. Here we report a novel ammonia production strategy, exemplified in an electrochemical...... lithium cycling process, which provides a pathway to sustainable ammonia synthesis via the ability to directly couple to renewable sources of electricity and can facilitate localized production. Whereas traditional aqueous electrochemical approaches are typically dominated by the hydrogen evolution...... reaction (HER), we are able to circumvent the HER by using a stepwise approach which separates the reduction of N2 from subsequent protonation to NH3, thus our synthesis method is predominantly selective for ammonia production. Density functional theory calculations for thermodynamic and diffusion energy...

Novel polymeric potassium complex: Its synthesis, structural characterization, photoluminescence and electrochemical properties

Energy Technology Data Exchange (ETDEWEB)

Ceyhan, Goekhan [Chemistry Department, K.Maras Suetcue Imam University, 46100 K.Maras (Turkey); Tuemer, Mehmet, E-mail: mtumer@ksu.edu.tr [Chemistry Department, K.Maras Suetcue Imam University, 46100 K.Maras (Turkey); Koese, Muhammet; McKee, Vickie [Chemistry Department, Loughborough University, LE11 3TU Leicestershire (United Kingdom)

2012-03-15

In this paper, we obtained a novel poly(vanillinato potassium) complex (PVP) as a single crystal and characterized by analytical and spectroscopic methods. A single crystal of the PVP was obtained from the acetone solution. X-ray structural data show that crystals contain polymeric K{sup +} complex of vanillin. Each potassium ion in the polymeric structure is identical and seven-coordinate, bonded to two methoxy, two phenoxy and three aldehyde oxygen atoms from four vaniline molecules. Two aldehyde oxygen atoms are bridging between potassium ions. It crystallizes in the monoclinic system, space group P2{sub 1}/c, with lattice parameters a=9.6215(10) A, b=17.4139(19) A, c=9.6119(10) A, {beta}=100.457(2) Degree-Sign and Z=4. Thermal properties of the PVP were investigated by TGA, DTA and DSC methods. The electrochemical properties of the complex were studied in different solvents and at various scan rates. The luminescence properties of the complex in different solvents and at different pH values have been investigated. The results show that the complex exhibits more efficient luminescence property in CH{sub 3}CN and n-butanol. - Highlights: Black-Right-Pointing-Pointer Novel polymeric potassium complex was prepared and fully characterized. Black-Right-Pointing-Pointer X-ray crystal structure of complex was reported. Black-Right-Pointing-Pointer Electrochemical properties of compound were investigated. Black-Right-Pointing-Pointer Thermal and DSC measurements of complex were examined.

Synthesis, characterization and electrochemical behavior of Sb-doped ZnO microsphere film

Energy Technology Data Exchange (ETDEWEB)

Li, Qian [Department of Materials Science and Engineering, State Key Laboratory of Silicon Materials, Cyrus Tang Center for Sensor Materials and Applications, Zhejiang University, Hangzhou, 310027 (China); Cheng, Kui, E-mail: chengkui@zju.edu.cn [Department of Materials Science and Engineering, State Key Laboratory of Silicon Materials, Cyrus Tang Center for Sensor Materials and Applications, Zhejiang University, Hangzhou, 310027 (China); Weng, Wenjian, E-mail: wengwj@zju.edu.cn [Department of Materials Science and Engineering, State Key Laboratory of Silicon Materials, Cyrus Tang Center for Sensor Materials and Applications, Zhejiang University, Hangzhou, 310027 (China); The Shanghai Institute of Ceramics, Chinese Academy of Sciences, 1295 Dingxi Road, Shanghai, 200050 (China); Du, Piyi; Han, Gaorong [Department of Materials Science and Engineering, State Key Laboratory of Silicon Materials, Cyrus Tang Center for Sensor Materials and Applications, Zhejiang University, Hangzhou, 310027 (China)

2013-10-01

Sb-doped ZnO microsphere film was fabricated by a carboxylate ion assisted hydrothermal route coupled with a post-calcination process. The structure, chemical composition and optical band gap of the Sb-doped ZnO microsphere film were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, inductively couple plasma optical emission spectroscopy and UV–visible spectrophotometry, and compared with the un-doped ZnO microsphere film. The results suggest that the formation of zinc–antimony tartrate complex species during hydrothermal growth is the key to realize Sb-doped ZnO microstructures, and the present hydrothermal method with post-calcination is an effective way to dope Sb into ZnO. Furthermore, the Sb-doped ZnO microsphere film based electrochemical biosensor exhibits a good sensing performance for the detection of hydrogen peroxide, with a sensitivity of 271 μA mM{sup −1} cm{sup −2} which is more than three times higher than that of the un-doped ZnO biosensor. - Highlights: • Sb-doped ZnO microsphere (SZM) films were grown by hydrothermal deposition. • Carboxylate ions were used to form complex during hydrothermal growth. • The formation of Zn–Sb tartrate complex is the key to realize SZM. • The biosensors based on SZM film are feasible and sensitive to detect H{sub 2}O{sub 2}. • The Sb doping could improve the electrochemical property of ZnO.

Polyfuran Conducting Polymers: Synthesis, Properties, and Applications.

OpenAIRE

González-Tejera, M.J.; Sánchez de la Blanca, Emilia; Carrillo Ramiro, Isabel

2008-01-01

In this review, polyfuran (PFu) synthesis methods and the nucleation mechanism; the electrochemical, structural, morphological, and magnetic properties of PFu; thermal behavior; theoretical calculations on PFu, as well as its applications reported to date, have been compiled. Not only PFu homopolymers have been reviewed, but also PFu co-polymers, PFu bipolymers, and PFu composites. The results are listed, discussed, and compared. It is hoped that this assembly of all the relevant data might e...

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

International Nuclear Information System (INIS)

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

2012-01-01

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

One-step hydrothermal synthesis and electrochemical performance of sodium-manganese-iron phosphate as cathode material for Li-ion batteries

Science.gov (United States)

Karegeya, Claude; Mahmoud, Abdelfattah; Vertruyen, Bénédicte; Hatert, Frédéric; Hermann, Raphaël P.; Cloots, Rudi; Boschini, Frédéric

2017-09-01

The sodium-manganese-iron phosphate Na2Mn1.5Fe1.5(PO4)3 (NMFP) with alluaudite structure was obtained by a one-step hydrothermal synthesis route. The physical properties and structure of this material were obtained through XRD and Mössbauer analyses. X-ray diffraction Rietveld refinements confirm a cationic distribution of Na+ and presence of vacancies in A(2)', Na+ and small amounts of Mn2+ in A(1), Mn2+ in M(1), 0.5 Mn2+ and Fe cations (Mn2+,Fe2+ and Fe3+) in M(2), leading to the structural formula Na2Mn(Mn0.5Fe1.5)(PO4)3. The particles morphology was investigated by SEM. Several reactions with different hydrothermal reaction times were attempted to design a suitable synthesis protocol of NMFP compound. The time of reaction was varied from 6 to 48 h at 220 °C. The pure phase of NMFP particles was firstly obtained when the hydrothermal reaction of NMFP precursors mixture was maintained at 220 °C for 6 h. When the reaction time was increased from 6 to 12, 24 and 48 h, the dandelion structure was destroyed in favor of NMFP micro-rods. The combination of NMFP (NMFP-6H, NMFP-12H, NMFP-24H and NMFP-48H) structure refinement and Mössbauer characterizations shows that the increase of the reaction time leads to the progressive increment of Fe(III) and the decrease of the crystal size. The electrochemical tests indicated that NMFP is a 3 V sodium intercalating cathode. The comparison of the discharge capacity evolution of studied NMFP electrode materials at C/5 current density shows different capacities of 48, 40, 34 and 34 mA h g-1 for NMFP-6H, NMFP-12H, NMFP-24H and NMFP-48H respectively. Interestingly, all samples show excellent capacity retention of about 99% during 50 cycles.

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

Science.gov (United States)

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.

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

International Nuclear Information System (INIS)

Yu Juanjuan; Hu Juncheng; Li Jinlin

2012-01-01

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

Synthesis and photo-electrochemical properties of spinel-ferrite-coated hematite for solar water splitting

Science.gov (United States)

Selvaraj, Seenivasan; Moon, Hee; Kim, Do-Heyoung

2018-01-01

Photo-electrochemical water splitting with hematite photo-anodes under solar irradiation has attracted considerable attention as regards the production of renewable hydrogen energy. However, many challenges remain unresolved, as the full contribution of the catalytic over-layers has not been fully realized. Herein, we incorporate uniform spinel nickel-ferrite over-layers in hematite photo-anodes to obtain an improved understanding of the associated intrinsic changes. We achieve a 1.5-mA/cm2 photo-current density at 1.23 VRHE (RHE: reversible hydrogen electrode) under one-sun illumination conditions, along with a negative shift of 200 mV in the onset potential, for NiFe2O4-coated Sn-doped hematite photo-anodes. Fundamental electrochemical analyses clearly show that the shift in the onset potential is predominantly due to the enhanced photo-voltage development inside the hematite, rather than being purely caused by the interfacial kinetics. These insights reveal a new direction for fundamental research on photo-anodes towards fabrication of more efficient photo-anode systems.

Carbonization-dependent nitrogen-doped hollow porous carbon nanospheres synthesis and electrochemical study for supercapacitors

Science.gov (United States)

Zhou, Lingyun; Xie, Guohong; Chen, Xiling

2018-05-01

In this paper, a nitrogen-doped hollow microporous carbon nanospheres was synthesized via the combination of hyper-crosslinking mediated self-assembly and further pyrolysis using polylactide-b-polystyrene (PLA-b-PS) copolymers and aniline monomers as precursor. The pore structure and the correlative electrochemical performance of nitrogen-doped hollow microporous carbon nanospheres were affected by the molar mass ratio of aniline and PS in block copolymers and the carbonization conditions. The electrochemical measurements results showed that the obtained PLA150-PS250-N4-900-10H sample with nitrogen content of 3.57% and the BET surface area of 945 m2 g-1 displays the best capacitance performance. At a current density of 1.0 Ag-1, the resultant specific capacitance is 250 Fg-1. In addition, it also exhibits high capacitance retention of 98% after charging-discharging 1500 times at 25 Ag-1. The results demonstrate the nitrogen-doped hollow microporous carbon nanospheres can be used as promising supercapacitor electrode materials for high performance energy storage devices.

Electrochemical Interphases for High-Energy Storage Using Reactive Metal Anodes

KAUST Repository

Wei, Shuya

2017-12-11

Conspectus Stable electrochemical interphases play a critical role in regulating transport of mass and charge in all electrochemical energy storage (EES) systems. In state-of-the-art rechargeable lithium ion batteries, they are rarely formed by design but instead spontaneously emerge from electrochemical degradation of electrolyte and electrode components. High-energy secondary batteries that utilize reactive metal anodes (e.g., Li, Na, Si, Sn, Al) to store large amounts of charge by alloying and/or electrodeposition reactions introduce fundamental challenges that require rational design in order to stabilize the interphases. Chemical instability of the electrodes in contact with electrolytes, morphological instability of the metal–electrolyte interface upon plating and stripping, and hydrodynamic-instability-induced electroconvection of the electrolyte at high currents are all known to cause metal electrode–electrolyte interfaces to continuously evolve in morphology, uniformity, and composition. Additionally, metal anodes undergo large changes in volume during lithiation and delithiation, which means that even in the rare cases where spontaneously formed solid electrode–electrolyte interphases (SEIs) are in thermodynamic equilibrium with the electrode, the SEI is under dynamic strain, which inevitably leads to cracking and/or rupture during extended battery cycling. There is an urgent need for interphases that are able to overcome each of these sources of instability with minimal losses of electrolyte and electrode components. Complementary chemical synthesis strategies are likewise urgently needed to create self-limited and mechanically durable SEIs that are able to flex and shrink to accommodate volume change. These needs are acute for practically relevant cells that cannot utilize large excesses of anode and electrolyte as employed in proof-of-concept-type experiments reported in the scientific literature. This disconnect between practical needs and

Hydrothermal Synthesis and Electrochemical Performance of Manganese Oxide (Na-OMS-2) Nanorods.

Science.gov (United States)

Zhang, Qing; Xu, Shan; Zheng, Hao; Luo, Zhaohui; Liu, Kang; Wang, Wei; Li, Guohua; Wang, Shiquan; Liu, Jianwen; Feng, Chuanqi

2017-02-01

Sodium octahedral molecular sieve nanorods (Na-OMS-2) were prepared through a facile hydrothermal method. The effects of reaction temperature and duration on particle sizes of the products were investigated. The electrochemical performance of samples was studied by constant current charge–discharge tests as cathode material for Li-ion batteries (LIBs). The initial discharge capacity of Na-OMS-2 is 123.4 mAh g−1 and the capacity retention was 123.9 mAh g−1 after 100 cycles. The result demonstrates that Na-OMS-2 cathode material behaves a good cycling stability.

Electrochemical thermodynamic measurement system

Science.gov (United States)

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

2009-09-29

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2014-01-01

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

Synthesis and characterization of the WxRuySez from the electrochemical reduction of oxygen and their possible application as electrode in fuel cell

International Nuclear Information System (INIS)

Ramirez R, S.D.

1995-01-01

In this communication the synthesis of the W 0.03 RuSe 0.47 O 0.3 from the transition metal carbonyl compounds and the chalcogenide in m Xylene, the chemical characterization of the novel material was performed by neutron activation analysis (NAA), using the TRIGA Mark III Reactor from the Nuclear Center of Mexico. The oxygen present in the material was determined by Rutherford Backscattering Spectrometry (RBS). Also the RuSe 5.7 y WSe 2 were synthesized and characterized by NAA. The electro kinetic oxygen reduction behaviour of the W 0.03 RuSe 0.47 O 0.3 deposited in glassy carbon was investigated in aqueous H 2 SO 4 0.5M. The rotating disk electrode electrochemical technique was used for determining the kinetic parameters: The reaction was of first order which implied that the rate determining step is the transfer of one electron, the Tafel slope was 0.115 V/decade; the electron transfer coefficient found was of 0.5, and the activation energy in the oxygen reduction reaction was 0.47 eV. (Author)

Electrochemical method for rapid synthesis of Zinc Pentacyanonitrosylferrate Nanotubes

Directory of Open Access Journals (Sweden)

Rogaieh Bargeshadi

2014-10-01

Full Text Available In this paper, a rapid and simple approach was developed for the preparation of zinc pentacyanonitrosylferrate nanotubes (ZnPCNF NTs within the cylindrical pores of anodic aluminum oxide (AAO template by electrochemical method. The AAO was fabricated in two steps anodizing from aluminum foil. The first anodization of aluminum foil was performed in 0.2 mol L-1 H2C2O4 followed by removal of the formed porous oxide film by a solution of 6 wt% of phosphoric acid. The second anodization step was then performed using the same conditions as the previous step. Scanning electron microscope (SEM and X-ray diffraction (XRD method were employed to characterize the resulting highly oriented uniform hollow tube array which its diameter was in the range of 25-75 nm depending on the applied voltage and the length of nanotubes was equal to the thickness of AAO which was about 2 m. The growth properties of the ZnPCNF NTs array film can be achieved by controlling the structure of the template and applied potential across the cell.

Microwave-polyol synthesis and electrocatalytic performance of Pt/graphene nanocomposites

International Nuclear Information System (INIS)

Liao, Chien-Shiun; Liao, Chien-Tsao; Tso, Ching-Yu; Shy, Hsiou-Jeng

2011-01-01

Highlights: · One-pot microwave-polyol synthesis of Pt/graphene electrocatalyst. · Simultaneous formation of Pt nanoparticles and reduction of graphene oxide. · Electrocatalytic activities depend on the morphology of the deposited Pt particles. · Dense dispersion of isolated Pt particles with high electrochemical active surface. · Few particle clusters of Pt have large number of active sites for methanol oxidation. - Abstract: Graphene oxide (GO) prepared by the modified Hummers method is used as a support in the formation of a Pt/GO nanocomposite electrocatalyst by microwave-polyol synthesis. The effects of microwave reaction times on particle size, dispersion, and electrocatalytic performance of Pt nanoparticles are studied using wide-angle X-ray diffractometery, Raman spectroscopy, transmission electron microscopy and three-electrode electrochemical measurements. The results indicate that Pt nanoparticles nucleation and growth occur, and the particles are uniformly deposited on the GO nanosheets within a short time. The maximum electrochemical active surface area 85.71 m 2 g -1 for a Pt/GO reaction time of 5 min, is a result of the deposition of a dense dispersion of small Pt particles. The highest methanol oxidation peak current density, I f , of 0.59 A mg -1 occurs for a Pt/GO reaction time of 10 min and is due to the formation of interconnecting Pt particles clusters. This novel Pt/GO nanocomposite electrocatalyst with high electrocatalytic activities has the potential for use as an anode material in fuel cells.

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

Science.gov (United States)

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 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 energy storage. Vol. 1. Fundamentals, aqueous storage batteries. Elektrochemische Energiespeicher. Bd. 1. Grundlagen, waessrige Akkumulatoren

Energy Technology Data Exchange (ETDEWEB)

Beck, F; Euler, K J

1984-01-01

Vol. 1 is a synthesis of electrochemical, battery-technical and energy industry aspects. The role of energy storage systems in the energy industry, e.g. in connection with a hydrogen technology, is discussed along with the thermodynamic, kinetic, materials-technical and process engineering fundamentals. ''Classic'' and new systems are described in full detail for the first time. Cyclisation and technical/economic criteria of selection are discussed. (orig./GG).

Electrochemical synthesis of mesoporous gold films toward mesospace-stimulated optical properties

Science.gov (United States)

Li, Cuiling; Dag, Ömer; Dao, Thang Duy; Nagao, Tadaaki; Sakamoto, Yasuhiro; Kimura, Tatsuo; Terasaki, Osamu; Yamauchi, Yusuke

2015-03-01

Mesoporous gold (Au) films with tunable pores are expected to provide fascinating optical properties stimulated by the mesospaces, but they have not been realized yet because of the difficulty of controlling the Au crystal growth. Here, we report a reliable soft-templating method to fabricate mesoporous Au films using stable micelles of diblock copolymers, with electrochemical deposition advantageous for precise control of Au crystal growth. Strong field enhancement takes place around the center of the uniform mesopores as well as on the walls between the pores, leading to the enhanced light scattering as well as surface-enhanced Raman scattering (SERS), which is understandable, for example, from Babinet principles applied for the reverse system of nanoparticle ensembles.

Ammonia synthesis at low temperatures

DEFF Research Database (Denmark)

Rod, Thomas Holm; Logadottir, Ashildur; Nørskov, Jens Kehlet

2000-01-01

have been carried out to evaluate its feasibility. The calculations suggest that it might be possible to catalytically produce ammonia from molecular nitrogen at low temperatures and pressures, in particular if energy is fed into the process electrochemically. (C) 2000 American Institute of Physics.......Density functional theory (DFT) calculations of reaction paths and energies for the industrial and the biological catalytic ammonia synthesis processes are compared. The industrial catalyst is modeled by a ruthenium surface, while the active part of the enzyme is modeled by a MoFe6S9 complex...

Tricobalt tetroxide nanoplate arrays on flexible conductive fabric substrate: Facile synthesis and application for electrochemical supercapacitors

Science.gov (United States)

Nagaraju, Goli; Ko, Yeong Hwan; Yu, Jae Su

2015-06-01

Tricobalt tetroxide (Co3O4) nanoplate arrays (NPAs) were synthesized on flexible conductive fabric substrate (FCFs) by a facile two-electrode system based electrochemical deposition method, followed by a simple heat treatment process. Initially, cobalt hydroxide (Co(OH)2) NPAs were electrochemically deposited on FCFs by applying an external voltage of -1.5 V for 30 min. Then, the Co3O4 NPAs on FCFs was obtained by thermal treatment of as-deposited Co(OH)2 NPAs on FCFs at 200 °C for 2 h. From the analysis of morphological and crystal properties, the Co3O4 NPAs were well integrated and uniformly covered over the entire surface of substrate with good crystallinity in the cubic phase. Additionally, the fabricated sample was directly used as a binder-free electrode to examine the feasibility for electrochemical supercapacitors using cyclic voltammetry and galvanic charge-discharge measurements in 1 M KOH electrolyte solution. The Co3O4 NPAs coated FCFs electrode exhibited a maximum specific capacitance of 145.6 F/g at a current density of 1 A/g and an excellent rate capability after 1000 cycles at a current density of 3 A/g. This facile fabrication method for integrating the Co3O4 nanostructures on FCFs could be a promising approach for advanced flexible electronic and energy-storage device applications.

Synthesis of new copper nanoparticle-decorated anchored type ligands: Applications as non-enzymatic electrochemical sensors for hydrogen peroxide

Energy Technology Data Exchange (ETDEWEB)

Ensafi, Ali A., E-mail: Ensafi@cc.iut.ac.ir; Zandi-Atashbar, N.; Ghiaci, M.; Taghizadeh, M.; Rezaei, B.

2015-02-01

In this work, copper nanoparticles (CuNPs) decorated on two new anchored type ligands were utilized to prepare two electrochemical sensors. These ligands are made from bonding amine chains to silica support including SiO{sub 2}–pro–NH{sub 2} (compound I) and SiO{sub 2}–pro–NH–cyanuric–NH{sub 2} (compound II). The morphology of synthesized CuNPs was characterized by transmission electron microscopy (TEM). The nano-particles were in the range of 13–37 nm with the average size of 23 nm. These materials were used to modify carbon paste electrode. Different electrochemical techniques, including cyclic voltammetry, electrochemical impedance spectroscopy and hydrodynamic chronoamperometry, were used to study the sensor behavior. These electrochemical sensors were used as a model for non-enzymatic detection of hydrogen peroxide (H{sub 2}O{sub 2}). To evaluate the abilities of the modified electrodes for H{sub 2}O{sub 2} detection, the electrochemical signals were compared in the absence and presence of H{sub 2}O{sub 2}. From them, two modified electrodes showed significant responses vs. H{sub 2}O{sub 2} addition. The amperograms illustrated that the sensors were selective for H{sub 2}O{sub 2} sensing with linear ranges of 5.14–1250 μmol L{sup −1} and 1.14–1120 μmol L{sup −1} with detection limits of 0.85 and 0.27 μmol L{sup −1} H{sub 2}O{sub 2}, sensitivities of 3545 and 11,293 μA mmol{sup −1} L and with response times less than 5 s for I/CPE and II/CPE, respectively. As further verification of the selected sensor, H{sub 2}O{sub 2} contained in milk sample was analyzed and the obtained results were comparable with the ones from classical control titration method. - Highlights: • Copper nanoparticles decorating on two new anchored type ligands were prepared. • Ligands are bonding to silica support as SiO{sub 2}–pro–NH{sub 2} and SiO{sub 2}–pro–NH–cyanuric–NH{sub 2}. • These materials were used as electrochemical sensors for H

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

International Nuclear Information System (INIS)

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

2016-01-01

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

Soft landing of bare PtRu nanoparticles for electrochemical reduction of oxygen.

Science.gov (United States)

Johnson, Grant E; Colby, Robert; Engelhard, Mark; Moon, Daewon; Laskin, Julia

2015-08-07

Magnetron sputtering of two independent Pt and Ru targets coupled with inert gas aggregation in a modified commercial source has been combined with soft landing of mass-selected ions to prepare bare 4.5 nm diameter PtRu nanoparticles on glassy carbon electrodes with controlled size and morphology for electrochemical reduction of oxygen in solution. Employing atomic force microscopy (AFM) it is shown that the nanoparticles bind randomly to the glassy carbon electrode at a relatively low coverage of 7 × 10(4) ions μm(-2) and that their average height is centered at 4.5 nm. Scanning transmission electron microscopy images obtained in the high-angle annular dark field mode (HAADF-STEM) further confirm that the soft-landed PtRu nanoparticles are uniform in size. Wide-area scans of the electrodes using X-ray photoelectron spectroscopy (XPS) reveal the presence of both Pt and Ru in atomic concentrations of ∼9% and ∼33%, respectively. Deconvolution of the high energy resolution XPS spectra in the Pt 4f and Ru 3d regions indicates the presence of both oxidized Pt and Ru. The substantially higher loading of Ru compared to Pt and enrichment of Pt at the surface of the nanoparticles is confirmed by wide-area analysis of the electrodes using time-of-flight medium energy ion scattering (TOF-MEIS) employing both 80 keV He(+) and O(+) ions. The activity of electrodes containing 7 × 10(4) ions μm(-2) of bare 4.5 nm PtRu nanoparticles toward the electrochemical reduction of oxygen was evaluated employing cyclic voltammetry (CV) in 0.1 M HClO4 and 0.5 M H2SO4 solutions. In both electrolytes a pronounced reduction peak was observed during O2 purging of the solution that was not evident during purging with Ar. Repeated electrochemical cycling of the electrodes revealed little evolution in the shape or position of the voltammograms indicating high stability of the nanoparticles supported on glassy carbon. The reproducibility of the nanoparticle synthesis and deposition was

Facile surfactant- and template-free synthesis and electrochemical properties of SnO{sub 2}/graphene composites

Energy Technology Data Exchange (ETDEWEB)

Li, Jing, E-mail: xy13787103391@126.com [School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010 (China); State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010 (China); Zhang, Xia, E-mail: zyx02090229@163.com [School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010 (China); State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010 (China); Guo, Jianqiang; Peng, Rufang [School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010 (China); State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010 (China); Xie, Ruishi [Analytical and Testing Center, Southwest University of Science and Technology, Mianyang 621010 (China); Huang, Yeju; Qi, Yongcheng [School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010 (China); State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010 (China)

2016-07-25

In this work, we demonstrate a facile and green hydrothermal process without using any surfactant or template to synthesize SnO{sub 2} nanoflowers (NFs)/graphene nanosheets (GNSs) composites as a high-performance electrode material for electric double layer capacitors (EDLCs). The crystal structure and morphology of the products were characterized by X-ray diffraction, scanning electron microscopy, and transition electron microscopy. The electrochemical properties were investigated by galvanostatic charge/discharge cycling and cycling voltammetry in a voltage range of −0.2–0.8 V. The results exhibit that the addition of GNSs did not change the tetragonal crystal structure of SnO{sub 2}, and the GNSs were successfully coated on the flower-like surface of SnO{sub 2}. The grain morphology of SnO{sub 2}@GNSs composites has a flower-like appearance suggesting excellent electrochemical properties which were confirmed by electrochemical techniques. Compared with the GNSs, the SnO{sub 2}@GNSs composites exhibit a high specific discharge capacitance of 126 F g{sup −1} at 0.2 A g{sup −1} and remains 98.2% after 2000 charge–discharge cycles. The combination of GNSs and SnO{sub 2} could significantly improve the electrical conductivity, enhance the interactions between GNSs and SnO{sub 2} NFs and provide more reaction sites, thereby resulting in improved electrochemical properties for the SnO{sub 2}@GNSs composites in contrast with the pristine GNSs sample. The high specific capacity and long stability make the SnO{sub 2}@GNSs nanocomposite as a electrode material for high-performance supercapacitors. - Highlights: • SnO{sub 2} nanoflowers (NFs)/Graphene nanosheets(GNSs) composites were prepared by a simple and rapid hydrothermal process. • The results show that the GNSs were homogeneously and tightly attached on the surface of SnO{sub 2} NFs. • The SnO{sub 2} NFs/GNSs composites electrode exhibited the enhanced capacitive performances than those of pure GNSs.

Phase-controlled synthesis of α-NiS nanoparticles confined in carbon nanorods for High Performance Supercapacitors

Science.gov (United States)

Sun, Chencheng; Ma, Mingze; Yang, Jun; Zhang, Yufei; Chen, Peng; Huang, Wei; Dong, Xiaochen

2014-11-01

A facile and phase-controlled synthesis of α-NiS nanoparticles (NPs) embedded in carbon nanorods (CRs) is reported by in-situ sulfurating the preformed Ni/CRs. The nanopore confinement by the carbon matrix is essential for the formation of α-NiS and preventing its transition to β-phase, which is in strong contrast to large aggregated β-NiS particles grown freely without the confinement of CRs. When used as electrochemical electrode, the hybrid electrochemical charge storage of the ultrasmall α-NiS nanoparticels dispersed in CRs is benefit for the high capacitor (1092, 946, 835, 740 F g-1 at current densities of 1, 2, 5, 10 A g-1, respectively.). While the high electrochemical stability (approximately 100% retention of specific capacitance after 2000 charge/discharge cycles) is attributed to the supercapacitor-battery electrode, which makes synergistic effect of capacitor (CRs) and battery (NiS NPs) components rather than a merely additive composite. This work not only suggests a general approach for phase-controlled synthesis of nickel sulfide but also opens the door to the rational design and fabrication of novel nickel-based/carbon hybrid supercapacitor-battery electrode materials.

Electrochemical analysis

International Nuclear Information System (INIS)

Hwang, Hun

2007-02-01

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

In situ one-pot synthesis of graphene–polyaniline nanofiber composite for high-performance electrochemical capacitors

International Nuclear Information System (INIS)

Jin, Yuhong; Fang, Mou; Jia, Mengqiu

2014-01-01

In this work, graphene–polyaniline nanofiber (G/PANI-F) composite is prepared through a new and one-pot method that includes the reduction of graphene oxide (GO) by aniline and then followed by in-situ polymerization. Aniline plays the two roles in this method: as a chemical reducing agent to reduce GO to graphene and as a monomer to prepare polyaniline nanofiber (PANI-F). Fourier transform infrared spectroscopy, X-ray diffraction, Raman spectra, X-ray photoelectron spectroscopy and transmission electron microscopy are employed to confirm that GO can be reduced by aniline and PANI-F can be deposited on the surface of graphene. The electrochemical properties of G/PANI-F composite electrode are measured by using cyclic voltammetry, galvanostatic charge–discharge test and electrochemical impedance spectroscopy. The G/PANI-F composite electrode exhibits enhanced specific capacitance of 965 F g −1 at 0.5 A g −1 and the capacity retention is 90% after 2000 cycles.

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

Energy Technology Data Exchange (ETDEWEB)

Han, Kun; Miao, Peng; Tang, Yuguo, E-mail: tangyg@sibet.ac.cn [Suzhou Institute of Biomedical Engineering and Technology, Chinese Academy of Sciences, Suzhou 215163 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Tong, Hui; Zhu, Xiaoli [Laboratory of Biosensing Technology, School of Life Sciences, Shanghai University, Shanghai 200444 (China); Liu, Tao; Cheng, Wenbo [Suzhou Institute of Biomedical Engineering and Technology, Chinese Academy of Sciences, Suzhou 215163 (China)

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.

High-performance symmetric electrochemical capacitor based on graphene foam and nanostructured manganese oxide

Directory of Open Access Journals (Sweden)

Abdulhakeem Bello

2013-08-01

Full Text Available We have fabricated a symmetric electrochemical capacitor with high energy and power densities based on a composite of graphene foam (GF with ∼80 wt% of manganese oxide (MnO2 deposited by hydrothermal synthesis. Raman spectroscopy and X-ray diffraction measurements showed the presence of nanocrystalline MnO2 on the GF, while scanning and transmission electron microscopies showed needle-like manganese oxide coated and anchored onto the surface of graphene. Electrochemical measurements of the composite electrode gave a specific capacitance of 240 Fg−1 at a current density of 0.1 Ag−1 for symmetric supercapacitors using a two-electrode configuration. A maximum energy density of 8.3 Whkg−1 was obtained, with power density of 20 kWkg−1 and no capacitance loss after 1000 cycles. GF is an excellent support for pseudo-capacitive oxide materials such as MnO2, and the composite electrode provided a high energy density due to a combination of double-layer and redox capacitance mechanisms.

Defect physics vis-à-vis electrochemical performance in layered mixed-metal oxide cathode materials

Science.gov (United States)

Hoang, Khang; Johannes, Michelle

Layered mixed-metal oxides with different compositions of (Ni,Co,Mn) [NCM] or (Ni,Co,Al) [NCA] have been used in commercial lithium-ion batteries. Yet their defect physics and chemistry is still not well understood, despite having important implications for the electrochemical performance. In this presentation, we report a hybrid density functional study of intrinsic point defects in the compositions LiNi1/3Co1/3Mn1/3O2 (NCM1/3) and LiNi1/3Co1/3Al1/3O2 (NCA1/3) which can also be regarded as model compounds for NCM and NCA. We will discuss defect landscapes in NCM1/3 and NCA1/3 under relevant synthesis conditions with a focus on the formation of metal antisite defects and its implications on the electrochemical properties and ultimately the design of NCM and NCA cathode materials.

Synthesis, characterization and electrochemical performance of core/shell structured carbon coated silicon powders for lithium ion battery negative electrodes

Directory of Open Access Journals (Sweden)

Tuğrul Çetinkaya

2017-06-01

Full Text Available Surface of nano silicon powders were coated with amorphous carbon by pyrolysis of polyacronitrile (PAN polymer. Microstructural characterization of amorphous carbon coated silicon powders (Si-C were carried out using scanning electron microscopy (SEM and thickness of carbon coating is defined by transmission electron microscopy (TEM. Elemental analyses of Si-C powders were performed using energy dispersive X-ray spectroscopy (EDS. Structural and phase characterization of Si-C composite powders were investigated using X-ray diffractometer (XRD and Raman spectroscopy. Produced Si-C powders were prepared as an electrode on the copper current collector and electrochemical tests were carried out using CR2016 button cells at 200 mA/g constant current density. According to electrochemical test results, carbon coating process enhanced the electrochemical performance by reducing the problems stem from volume change and showed 770 mAh/g discharge capacity after 30 cycles.

Pyro-synthesis of functional nanocrystals.

Science.gov (United States)

Gim, Jihyeon; Mathew, Vinod; Lim, Jinsub; Song, Jinju; Baek, Sora; Kang, Jungwon; Ahn, Docheon; Song, Sun-Ju; Yoon, Hyeonseok; Kim, Jaekook

2012-01-01

Despite nanomaterials with unique properties playing a vital role in scientific and technological advancements of various fields including chemical and electrochemical applications, the scope for exploration of nano-scale applications is still wide open. The intimate correlation between material properties and synthesis in combination with the urgency to enhance the empirical understanding of nanomaterials demand the evolution of new strategies to promising materials. Herein we introduce a rapid pyro-synthesis that produces highly crystalline functional nanomaterials under reaction times of a few seconds in open-air conditions. The versatile technique may facilitate the development of a variety of nanomaterials and, in particular, carbon-coated metal phosphates with appreciable physico-chemical properties benefiting energy storage applications. The present strategy may present opportunities to develop "design rules" not only to produce nanomaterials for various applications but also to realize cost-effective and simple nanomaterial production beyond lab-scale limitations.

Design and synthesis of hierarchical MnO2 nanospheres/carbon nanotubes/conducting polymer ternary composite for high performance electrochemical electrodes.

Science.gov (United States)

Hou, Ye; Cheng, Yingwen; Hobson, Tyler; Liu, Jie

2010-07-14

For efficient use of metal oxides, such as MnO(2) and RuO(2), in pseudocapacitors and other electrochemical applications, the poor conductivity of the metal oxide is a major problem. To tackle the problem, we have designed a ternary nanocomposite film composed of metal oxide (MnO(2)), carbon nanotube (CNT), and conducting polymer (CP). Each component in the MnO(2)/CNT/CP film provides unique and critical function to achieve optimized electrochemical properties. The electrochemical performance of the film is evaluated by cyclic voltammetry, and constant-current charge/discharge cycling techniques. Specific capacitance (SC) of the ternary composite electrode can reach 427 F/g. Even at high mass loading and high concentration of MnO(2) (60%), the film still showed SC value as high as 200 F/g. The electrode also exhibited excellent charge/discharge rate and good cycling stability, retaining over 99% of its initial charge after 1000 cycles. The results demonstrated that MnO(2) is effectively utilized with assistance of other components (fFWNTs and poly(3,4-ethylenedioxythiophene)-poly(styrenesulfonate) in the electrode. Such ternary composite is very promising for the next generation high performance electrochemical supercapacitors.

Hydrogen storage material, electrochemically active material, electrochemical cell and electronic equipment

NARCIS (Netherlands)

2008-01-01

The invention relates to a hydrogen storage material comprising an alloy of magnesium. The invention further relates to an electrochemically active material and an electrochemical cell provided with at least one electrode comprising such a hydrogen storage material. Also, the invention relates to

Electrochemical potassium-ion intercalation in NaxCoO2: a novel cathode material for potassium-ion batteries.

Science.gov (United States)

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.

Graphene oxide directed in-situ synthesis of Prussian blue for non-enzymatic sensing of hydrogen peroxide released from macrophages

Energy Technology Data Exchange (ETDEWEB)

Qiu, Weiwei; Zhu, Qionghua; Gao, Fei; Gao, Feng [College of Chemistry and Environment, Fujian Province Key Laboratory of Morden Analytical Science and Separation Technology, Minnan Normal University, Zhangzhou 363000 (China); Huang, Jiafu; Pan, Yutian [College of Biological Science and Technology, Minnan Normal University, Zhangzhou 363000 (China); Wang, Qingxiang, E-mail: axiang236@126.com [College of Chemistry and Environment, Fujian Province Key Laboratory of Morden Analytical Science and Separation Technology, Minnan Normal University, Zhangzhou 363000 (China)

2017-03-01

A novel electrochemical non-enzymatic hydrogen peroxide (H{sub 2}O{sub 2}) sensor has been developed based on Prussian blue (PB) and electrochemically reduced graphene oxide (ERGO). The GO was covalently modified on glassy carbon electrode (GCE), and utilized as a directing platform for in-situ synthesis of electroactive PB. Then the GO was electrochemically treated to reduction form to improve the effective surface area and electroactivity of the sensing interface. The fabrication process was characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and atomic force microscopy (AFM). The results showed that the rich oxygen containing groups play a crucial role for the successful synthesis of PB, and the obtained PB layer on the covalently immobilized GO has good stability. Electrochemical sensing assay showed that the modified electrode had tremendous electrocatalytic property for the reduction of H{sub 2}O{sub 2}. The steady-state current response increased linearly with H{sub 2}O{sub 2} concentrations from 5 μM to 1 mM with a fast response time (less than 3 s). The detection limit was estimated to be 0.8 μM. When the sensor was applied for determination of H{sub 2}O{sub 2} released from living cells of macrophages, satisfactory results were achieved. - Highlights: • Covalent method was applied for immobilization of GO on glassy carbon electrode. • GO directed in-situ synthesis of electroactive PB. • PB-ERGO composite shows high electrocatalytic activity toward H{sub 2}O{sub 2}. • The modified biosensor is capable of detecting H{sub 2}O{sub 2} released from living macrophages.

Graphene-Paper Based Electrochemical Sensors

DEFF Research Database (Denmark)

Zhang, Minwei; Halder, Arnab; Cao, Xianyi

2017-01-01

in electrochemical sensors and energy technologies amongothers. In this chapter, we present some examples to overview recent advances in theresearch and development of two-dimensional (2D) graphene papers as new materialsfor electrochemical sensors. The chapter covers the design, fabrication, functionalizationand...... functionalization ofgraphene papers with polymer and nanoscale functional building blocks for electrochemical-sensing purposes. In terms of electrochemical-sensing applications, the emphasis ison enzyme-graphene and nanoparticle-graphene paper-based systems for the detectionof glucose. We finally conclude...

Nano-TiO_2 coatings on aluminum surfaces by aerosol flame synthesis

International Nuclear Information System (INIS)

Liberini, Mariacira; De Falco, Gianluigi; Scherillo, Fabio; Astarita, Antonello; Commodo, Mario; Minutolo, Patrizia; D'Anna, Andrea; Squillace, Antonino

2016-01-01

Aluminum alloys are widely used in the aeronautic industry for their high mechanical properties; however, because they are very sensitive to corrosion, surface treatments are often required. TiO_2 has excellent resistance to oxidation and it is often used to improve the corrosion resistance of aluminum surfaces. Several coating procedures have been proposed over the years, which are in some cases expensive in terms of production time and amount of deposited material. Moreover, they can damage aluminum alloys if thermal treatments are required. In this paper, a one-step method for the coating of aluminum surfaces with titania nanoparticles is presented. Narrowly sized, TiO_2 nanoparticles are synthesized by flame aerosol and directly deposited by thermophoresis onto cold plates of aluminum AA2024. Submicron coatings of different thicknesses are obtained from two flame synthesis conditions by varying the total deposition time. A fuel-lean synthesis condition was used to produce 3.5 nm pure anatase nanoparticles, while a mixture of rutile and anatase nanoparticles having 22 nm diameter — rutile being the predominant phase —, was synthesized in a fuel-rich condition. Scanning electron microscopy is used to characterize morphology of titania films, while coating thickness is measured by confocal microscopy measurements. Electrochemical impedance spectroscopy is used to evaluate corrosion resistance of coated aluminum substrates. Results show an improvement of the electrochemical behavior of titania coated surfaces as compared to pristine aluminum surfaces. The best results are obtained by covering the substrates with 3.5 nm anatase-phase nanoparticles and with lower deposition times, that assure a uniform surface coating. - Highlights: • Nanosized TiO_2 particles produced by aerosol flame synthesis • Coatings of aluminum substrates with TiO_2 nanoparticles by thermophoretic deposition in flames • Thickness measurement by confocal microscopy • Improvement of

Synthesis of [14α-methyl-3H]-24,25-dihydrolanosterol

International Nuclear Information System (INIS)

DeKeczer, S.; Kertesz, D.; Parnes, H.

1993-01-01

We describe the first synthesis of isomerically pure title compound (6) at high specific activity. This required the development of a convenient, regiospecific synthesis of the δ 8(9) -15-ketone and subsequent alkylation with methyl-[ 3 H 3 ]iodide. A key step in our procedure was the use of an electrochemical reduction of the intermediate [14α-methyl- 3 H]-15-oxo-dihydrolanosterol. This process was effected cleanly and in high yield to give (6), an important assay tool in the search for cholesterol lowering agents. This approach was found to be significantly superior to the Wolff-Kishner reduction of the corresponding 3-benzoate. (Author)

Synthesis, characterization and electrochemical performances of new antimony-containing graphite compounds used as anodes for lithium-ion batteries

International Nuclear Information System (INIS)

Dailly, A.; Willmann, P.; Billaud, D.

2002-01-01

Graphite intercalation intercalated with metal alloys able to alloy reversibly lithium constitute a large set of new anodic materials for lithium-ion batteries of significantly improved reversible capacities. Especially, graphite intercalated with cesium-antimony alloys can be used as materials for anodes in lithium-ion batteries. Electrochemical insertion of lithium in such chemically modified precursors shows that lithium both intercalates in the empty van der Waals spaces of graphite and alloys reversibly with antimony. The total electrochemical reversible capacities, measured between 0 and 2 V vs Li + /Li, close to 700 mAh g -1 have been currently obtained

Cobalt-Doped Nickel Phosphite for High Performance of Electrochemical Energy Storage.

Science.gov (United States)

Li, Bing; Shi, Yuxin; Huang, Kesheng; Zhao, Mingming; Qiu, Jiaqing; Xue, Huaiguo; Pang, Huan

2018-03-01

Compared to single metallic Ni or Co phosphides, bimetallic Ni-Co phosphides own ameliorative properties, such as high electrical conductivity, remarkable rate capability, upper specific capacity, and excellent cycle performance. Here, a simple one-step solvothermal process is proposed for the synthesis of bouquet-like cobalt-doped nickel phosphite (Ni 11 (HPO 3 ) 8 (OH) 6 ), and the effect of the structure on the pseudocapacitive performance is investigated via a series of electrochemical measurements. It is found that when the cobalt content is low, the glycol/deionized water ratio is 1, and the reaction is under 200 °C for 20 h, the morphology of the sample is uniform and has the highest specific surface area. The cobalt-doped Ni 11 (HPO 3 ) 8 (OH) 6 electrode presents a maximum specific capacitance of 714.8 F g -1 . More significantly, aqueous and solid-state flexible electrochemical energy storage devices are successfully assembled. The aqueous device shows a high energy density of 15.48 mWh cm -2 at the power density of 0.6 KW cm -2 . The solid-state device shows a high energy density of 14.72 mWh cm -2 at the power density of 0.6 KW cm -2 . These excellent performances confirm that the cobalt-doped Ni 11 (HPO 3 ) 8 (OH) 6 are promising materials for applications in electrochemical energy storage devices. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electrochemical synthesis of novel {pi}-extended phenoxazine derivatives of porphyrincatecholes

Energy Technology Data Exchange (ETDEWEB)

Osati, Samira; Davarani, Saied Saeed Hosseiny [Department of Chemistry, Faculty of Science, Shahid Beheshti University, G.C, Evin, 1983963113 Tehran (Iran, Islamic Republic of); Safari, Nasser, E-mail: n-safari@cc.sbu.ac.ir [Department of Chemistry, Faculty of Science, Shahid Beheshti University, G.C, Evin, 1983963113 Tehran (Iran, Islamic Republic of); Banitaba, Mohammad Hossein [Department of Chemistry, Faculty of Science, Shahid Beheshti University, G.C, Evin, 1983963113 Tehran (Iran, Islamic Republic of)

2011-10-30

Three new functionalized phenoxazine-catechol porphyrins 7a-c have been synthesized by a green one-pot method and structurally characterized by spectroscopic analysis. The electro-oxidation of 5,10,15,20-tetrakis(2,3-dihydroxyphenyl) porphyrins(1a-c) with four catechol units in the presence of 2-aminophenol 8 as bidentate nucleophile has been done and phenoxazine rings have been formed by intermolecular and intramolecular Michael addition reactions. Spectroscopic characterization and voltammetry results have allowed us to propose four independent ECEC mechanisms for the electrochemical oxidation pathway. The functionalization of the porphyrins affected their photophysical properties. Expansion of the UV-vis spectrum range and the decrease of the fluorescence intensity of the products would support the energy transfer between the porphyrin core excited states to the four substitutions as the electron acceptor subunits. SEM images indicate that this method produces regularly shaped manganese porphyrin nano-particles 7c that possess a cubic nano structure.

Synthesis of cationic star polymers by simplified electrochemically mediated ATRP

Directory of Open Access Journals (Sweden)

P. Chmielarz

2016-10-01

Full Text Available Cyclodextrin-based cationic star polymers were synthesized using β-cyclodextrin (β-CD core, and 2-(dimethylamino ethyl methacrylate (DMAEMA as hydrophilic arms. Star-shaped polymers were prepared via a simplified electrochemically mediated ATRP (seATRP under potentiostatic and galvanostatic conditions. The polymerization results showed molecular weight (MW evolution close to theoretical values, and maintained narrow molecular weight distribution (MWD of obtained stars. The rate of the polymerizations was controlled by applying more positive potential values thereby suppressing star-star coupling reactions. Successful chain extension of the ω-functional arms with a hydrophobic n-butyl acrylate (BA formed star block copolymers and confirmed the living nature of the β-CD-PDMAEMA star polymers prepared by seATRP. Novelty of this work is that the β-CD-PDMAEMA-b-PBA cationic star block copolymers were synthesized for the first time via seATRP procedure, utilizing only 40 ppm of catalyst complex. The results from 1H NMR spectral studies support the formation of cationic star (copolymers.

High-performance lithium-rich layered oxide materials: Effects of chelating agents on microstructure and electrochemical properties

International Nuclear Information System (INIS)

Li, Lingjun; Xu, Ming; Chen, Zhaoyong; Zhou, Xiang; Zhang, Qiaobao; Zhu, Huali; Wu, Chun; Zhang, Kaili

2015-01-01

The mechanisms and effects of three typical chelating agents, namely glucose, citric acid and sucrose on the sol-gel synthesis process, electrochemical degradation and structural evolution of 0.5Li 2 MnO 3 ·0.5LiNi 0.5 Co 0.2 Mn 0.3 O 2 (LLMO) materials are systematically compared for the first time. X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy and high-resolution transmission electron microscopy analysis indicate that the sample synthesized from sucrose owns well structure, homogenous distribution, low Ni 3+ concentration and good surface structural stability during cycling, respectively. Electrochemical tests further prove that the LLMO material obtained from sucrose maintains 258.4 mAh g −1 with 94.8% capacity retention after 100 cycles at 0.2 C. The superior electrochemical performance can be ascribed to the exceptional complexing mechanism of sucrose, compared to those of the glucose and citric acid. Namely, one mole sucrose can be hydrolyzed into two different monosaccharides and further chelates three M (Li, Ni, Co and Mn) ions to form a more uniform ion-chelated matrix during sol-gel process. This discovery is an important step towards understanding the selection criterion of chelating agents for sol-gel method, that chelating agent with excellent complexing capability is beneficial to the distribution, structural stability and electrochemical properties of advanced lithium-rich layered materials

Metal Phosphides and Phosphates-based Electrodes for Electrochemical Supercapacitors.

Science.gov (United States)

Li, Xin; Elshahawy, Abdelnaby M; Guan, Cao; Wang, John

2017-10-01

Phosphorus compounds, such as metal phosphides and phosphates have shown excellent performances and great potential in electrochemical energy storage, which are demonstrated by research works published in recent years. Some of these metal phosphides and phosphates and their hybrids compare favorably with transition metal oxides/hydroxides, which have been studied extensively as a class of electrode materials for supercapacitor applications, where they have limitations in terms of electrical and ion conductivity and device stability. To be specific, metal phosphides have both metalloid characteristics and good electric conductivity. For metal phosphates, the open-framework structures with large channels and cavities endow them with good ion conductivity and charge storage capacity. In this review, we present the recent progress on metal phosphides and phosphates, by focusing on their advantages/disadvantages and potential applications as a new class of electrode materials in supercapacitors. The synthesis methods to prepare these metal phosphides/phosphates are looked into, together with the scientific insights involved, as they strongly affect the electrochemical energy storage performance. Particular attentions are paid to those hybrid-type materials, where strong synergistic effects exist. In the summary, the future perspectives and challenges for the metal phosphides, phosphates and hybrid-types are proposed and discussed. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electrochemical force microscopy

Energy Technology Data Exchange (ETDEWEB)

Kalinin, Sergei V.; Jesse, Stephen; Collins, Liam F.; Rodriguez, Brian J.

2017-01-10

A system and method for electrochemical force microscopy are provided. The system and method are based on a multidimensional detection scheme that is sensitive to forces experienced by a biased electrode in a solution. The multidimensional approach allows separation of fast processes, such as double layer charging, and charge relaxation, and slow processes, such as diffusion and faradaic reactions, as well as capturing the bias dependence of the response. The time-resolved and bias measurements can also allow probing both linear (small bias range) and non-linear (large bias range) electrochemical regimes and potentially the de-convolution of charge dynamics and diffusion processes from steric effects and electrochemical reactivity.

Electrochemical oxidation of 3,5-di-tert-butylcatechol: Synthesis and characterization of the formed ortho-benzoquinhydrone derivative

International Nuclear Information System (INIS)

Nematollahi, D.; Shayani-Jam, H.

2006-01-01

Electrochemical oxidation of 3,5-di-tert-butylcatechol (1) has been studied in ethanol/water mixtures by means of cyclic voltammetry and controlled-potential coulometry. The results revealed that 3,5-di-tert-butyl-1,2-benenzoquinone (2) derived from oxidation of 3,5-di-tert-butylcatechol participate in noncovalently linked interactions with 1 converted to an ortho-benzoquinhydrone (3). The structure of 3 was characterized by MS, IR, 1 H NMR and 13 C NMR. The 1 H NMR studies reveal that the benzoquinhydrone complex 3 is stabilized by one H-bonding interaction. In this work we derived a novel ortho-bezoquinhydrone type complex (3) based on electrochemical oxidation of 3,5-di-tert-butylcatechol at carbon electrode in an undivided cell

Study of chemical and electrochemical properties of some elements in molten NaAlCl

International Nuclear Information System (INIS)

Bermond, Alain

1976-01-01

We describe a study of the electrochemical and chemical properties in molten mixtures of Aluminium Chloride-Sodium chloride, at 210 deg. C and the concept of acidity, related to chloride activity, is previously summarized. In a first part, the study of Mercury and Cadmium by means of electro-analytical techniques, states the Hg 2+ 2 , Hg 2+ , Cd 2+ 2 and Cd 2+ ions and their acid properties. Some diagrams Equilibrium potential vs acidity are the synthesis of these results. In a second part, it is shown that a nickel electrode is an indicator of the presence of oxide ions; from interpretation of electrochemical results, O 2 appears to behave, in terms of the chloro-acido-basicity concept, as a strong di-base, giving the solvated form AlOCl - 2 , or a strong tri-base giving AlOCl. A saturation effect by Al 2 O 3 appears when the oxide concentration is increased; the solubility of Al 2 O 3 versus acidity is determined from the electrochemical results. In a third part, results for the Ni/Ni(II) or HCl/H 2 O systems are related to dissolved oxide ion presence in chloroaluminate melts; elimination of oxide ions, through H 2 O formation, by reaction with HCl is noteworthy. (author) [fr

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

Science.gov (United States)

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

2015-10-07

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

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

Science.gov (United States)

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

2013-05-01

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

Electrochemical Supercapacitor Electrodes from Sponge-like Graphene Nanoarchitectures with Ultrahigh Power Density.

Science.gov (United States)

Xu, Zhanwei; Li, Zhi; Holt, Chris M B; Tan, Xuehai; Wang, Huanlei; Amirkhiz, Babak Shalchi; Stephenson, Tyler; Mitlin, David

2012-10-18

We employed a microwave synthesis process of cobalt phthalocyanine molecules templated by acid-functionalized multiwalled carbon nanotubes to create three-dimensional sponge-like graphene nanoarchitectures suited for ionic liquid-based electrochemical capacitor electrodes that operate at very high scan rates. The sequential "bottom-up" molecular synthesis and subsequent carbonization process took less than 20 min to complete. The 3D nanoarchitectures are able to deliver an energy density of 7.1 W·h kg(-1) even at an extra high power density of 48 000 W kg(-1). In addition, the ionic liquid supercapacitor based on this material works very well at room temperature due to its fully opened structures, which is ideal for the high-power energy application requiring more tolerance to temperature variation. Moreover, the structures are stable in both ionic liquids and 1 M H2SO4, retaining 90 and 98% capacitance after 10 000 cycles, respectively.

Evaluation of the aniline chemical oxidation process using multiple simultaneous electrochemical responses

International Nuclear Information System (INIS)

Cristovan, Fernando H.; Lemos, Sherlan G.; Santos, Janaina S.; Trivinho-Strixino, Francisco; Pereira, Ernesto C.; Mattoso, Luiz H.C.; Kulkarni, Rashmi; Manohar, Sanjeev K.

2010-01-01

In this paper we show the simultaneous evaluation of the electrochemical impedance, the open circuit potential and the mass variation of the polyaniline deposited on a metal substrate during chemical oxidation of aniline. We detected that the final properties of the polymer could be practically defined after the inflection point of the potential profile. Considering a series connection of R and C, impedance Z was decomposed into the resistive and capacitive components. The resistivity and permittivity show a slight change after the inflection point in the potential profile. Impedance data and mass changes during synthesis also contributed to a better definition of the induction period. We described the system as whole, which relates to an electronic transport and to an electronic charge storage process. Although very simple, this model helps us to interpret and correlate different techniques to explain the results. In addition, we demonstrated that the in situ evaluation of the parameters described above offers new insights on the chemical synthesis mechanism of polyaniline.

Synthesis of fully and partially sulfonated polyanilines derived from ortanilic acid: An electrochemical and electromicrogravimetric study

International Nuclear Information System (INIS)

Cano Marquez, Abraham Guadalupe; Torres Rodriguez, Luz Maria; Montes Rojas, Antonio

2007-01-01

The electrochemical polymerization of 2-aminobenzene sulfonic acid, also called ortanilic acid (o-ASA), on a gold electrode precoated with polyaniline (PANI), has been carried out. We proved that the electropolymerization of o-ASA is enhanced on PANI electrodes, resulting in thicker films obtained in aqueous media at room temperature. The electrosynthesized film (P(o-ASA)) was characterized by cyclic voltammetry, FTIR and nuclear magnetic resonance. The compensation of P(o-ASA) charge was evaluated using electrochemical quartz crystal microbalance combined with cyclic voltammetry, which showed that the electroneutralization process mainly involves cations. Additionally, copolymers of aniline and o-ASA were electrosynthesized, using a metallic electrode modified with PANI also as a working electrode. The degree of sulfanation of copolymers has been modulated with the proportions of monomers in the electrosynthesis solution. The studies reveal a more important participation of cations in fully sulfonated polyaniline than in partially sulfonated polyaniline

Synthesis and electrochemical characteristics of Sn-Sb-Ni alloy composite anode for Li-ion rechargeable batteries

International Nuclear Information System (INIS)

Guo Hong; Zhao Hailei; Jia Xidi; Qiu Weihua; Cui Fenge

2007-01-01

Micro-scaled Sn-Sb-Ni alloy composite was synthesized from oxides of Sn, Sb and Ni via carbothermal reduction. The phase composition and electrochemical properties of the Sn-Sb-Ni alloy composite anode material were studied. The prepared alloy composite electrode exhibits a high specific capacity and a good cycling stability. The lithiation capacity was 530 mAh g -1 in the first cycle and maintained at 370-380 mAh g -1 in the following cycles. The good electrochemical performance may be attributed to its relatively large particle size and multi-phase characteristics. The former reason leads to the lower surface impurity and thus the lower initial capacity loss, while the latter results in a stepwise lithiation/delithiation behavior and a smooth volume change of electrode in cycles. The Sn-Sb-Ni alloy composite material shows a good candidate anode material for the rechargeable lithium ion batteries

Review on the progress in synthesis and application of magnetic carbon nanocomposites

Science.gov (United States)

Zhu, Maiyong; Diao, Guowang

2011-07-01

This review focuses on the synthesis and application of nanostructured composites containing magnetic nanostructures and carbon-based materials. Great progress in fabrication of magnetic carbon nanocomposites has been made by developing methods including filling process, template-based synthesis, chemical vapor deposition, hydrothermal/solvothermal method, pyrolysis procedure, sol-gel process, detonation induced reaction, self-assembly method, etc. The applications of magnetic carbon nanocomposites expanded to a wide range of fields such as environmental treatment, microwave absorption, magnetic recording media, electrochemical sensor, catalysis, separation/recognization of biomolecules and drug delivery are discussed. Finally, some future trends and perspectives in this research area are outlined.

Electrochemical characterization of core@shell CoFe{sub 2}O{sub 4}/Au composite

Energy Technology Data Exchange (ETDEWEB)

Carla, Francesco [' Ugo Schiff' , Universita degli Studi di Firenze, Dipartimento di Chimica (Italy); Campo, Giulio; Sangregorio, Claudio; Caneschi, Andrea; Julian Fernandez, Cesar de; Cabrera, Lourdes I., E-mail: lourisa_cabrera@yahoo.com [Universita degli Studi di Firenze, Laboratorio di Magnetismo Molecolare, INSTM, Dipartimento di Chimica (Italy)

2013-08-15

In this paper, we address the synthesis and characterization of the core@shell composite magneto-plasmonic cobalt ferrite-gold (Co-ferrite/Au) nanosystem. The synthesis Co-ferrite/Au nanocomposite is not obvious, hence it was of interest to generate it in a simple straightforward method. Co-ferrite/Au nanocomposite was generated by synthesizing first by thermal decomposition Co-ferrite nanoparticles (NPs). On a second step, ionic gold (Au{sup 3+}) was reduced at the surface of Co-ferrite NPs by ultrasound, to obtain the metallic Au shell. The characterization of the nanomaterial was achieved by microscopy, spectroscopy, and performing magnetic measurements. However, what is attractive about our work is the use of electrochemical techniques as analytical tools. The key technique was cyclic voltammetry, which provided information about the nature and structure of the nanocomposite, allowing us to confirm the core@shell structure.

Materials for electrochemical capacitors

Science.gov (United States)

Simon, Patrice; Gogotsi, Yury

2008-11-01

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

Electrochemical reduction of NOx

DEFF Research Database (Denmark)

Traulsen, Marie Lund

NO and NO2 (collectively referred to as NOx) are air pollutants, and the largest single contributor to NOx pollution is automotive exhaust. This study investigates electrochemical deNOx, a technology which aims to remove NOx from automotive diesel exhaust by electrochemical reduction of NOx to N2...... and O2. The focus in this study is on improving the activity and selectivity of solid oxide electrodes for electrochemical deNOx by addition of NOx storage compounds to the electrodes. Two different composite electrodes, La0.85Sr0.15MnO3-δ-Ce0.9Gd0.1O1.95 (LSM15-CGO10) and La0.85Sr0.15FeO3-δ-Ce0.9Gd0.1O......1.95 (LSF15-CGO10), have been investigated in combination with three different NOx storage compounds: BaO, K2O and MnOx. The main focus in the investigation has been on conversion measurements and electrochemical characterization, the latter by means of electrochemical impedance spectroscopy...

Study on Electrochemical Performance of Carbonnanotubes/Fey 04 Composite Electrode Material

Directory of Open Access Journals (Sweden)

WANG Fang--yong

2017-02-01

Full Text Available For single super capacitor materials，each material has its own unique advantages and defects. In this paper, the synthesis of complex multi walled carbon nanotubes with Fe304 nanoparticles by simple hydrothermal method. Composite performance for Fe3 OQ nanoparticles adsorbed on carbon nano tube wall composed of reticular structure morphology. Synergy of two component，provides the binary nanometer compound larger specific capacity， excellent properties and good cycle stability. The experimental results proved that the improvement effects of CNT carbon materials on the electrochemical properties of pseudocapacitive electrode material，and CNT/Fe3 OQ nano- composites applied to supercapacitor electrode material.

Synthesis of nitrogen doped microporous carbons prepared by activation-free method and their high electrochemical performance

Energy Technology Data Exchange (ETDEWEB)

Kim, Ki-Seok [Department of Chemistry, Inha University, Incheon 402-751 (Korea, Republic of); Park, Soo-Jin, E-mail: sjpark@inha.ac.kr [Department of Chemistry, Inha University, Incheon 402-751 (Korea, Republic of)

2011-11-30

Graphical abstract: This describes the increase of specific capacitance in hybrid electrodes as a function of melamine content. Display Omitted Highlights: > For N-enriched hybrid carbons, co-precursors, PVDF/melamine composites, were used. > Microporous carbons were formed by only carbonization without chemical activation. > The nitrogen content of microporous carbons was controlled by melamine content. > N-doped carbons showed higher specific capacitance compared to microporous carbons. > It was attributed to the easy electron transfer and pseudocapacitance. - Abstract: Nitrogen-doped microporous carbons (N-MCs) were prepared by the carbonization of the polyvinylidene fluoride (PVDF)/melamine mixture without chemical activation. The electrochemical performance of the N-MCs was investigated as a function of PVDF/melamine ratio. It was found that, without additional activation, the N-MCs had a high specific surface area (greater than 560 m{sup 2}/g) because of the micropore formation by the release of fluorine groups. In addition, although the specific surface area decreased, nitrogen groups were increased with increasing melamine content, leading to an enhanced electrochemical performance. Indeed, the N-MCs showed a better electrochemical performance than that of microporous carbons (MCs) prepared by PVDF alone, and the highest specific capacitance (310 F/g) was obtained at a current density of 0.5 A/g, as compared to a value of 248 F/g for MCs. These results indicate that the microporous features of N-MC lead to feasible ion transfer during charge/discharge duration and the presence of nitrogen groups as strong electron donor on the N-MC electrode in electrolyte could provide a pseudocapacitance by the redox reaction.

Electrochemical process for the manufacturing of titanium alloy matrix composites

Directory of Open Access Journals (Sweden)

V. Soare

2009-07-01

Full Text Available The paper presents a new method for precursors’ synthesis of titanium alloys matrix composites through an electrochemical process in molten calcium chloride. The cathode of the cell was made from metallic oxides powders and reinforcement ceramic particles, which were pressed and sintered into disk form and the anode from graphite. The process occurred at 850 °C, in two stages, at 2,7 / 3,2 V: the ionization of the oxygen in oxides and the reduction with calcium formed by electrolysis of calcium oxide fed in the electrolyte. The obtained composite precursors, in a form of metallic sponge, were consolidated by pressing and sintering. Chemical and structural analyses on composites samples were performed.

Facile solvothermal synthesis of a graphene nanosheet-bismuth oxide composite and its electrochemical characteristics

International Nuclear Information System (INIS)

Wang Huanwen; Hu Zhongai; Chang Yanqin; Chen Yanli; Lei Ziqiang; Zhang Ziyu; Yang Yuying

2010-01-01

This work demonstrates a novel and facile route for preparing graphene-based composites comprising of metal oxide nanoparticles and graphene. A graphene nanosheet-bismuth oxide composite as electrode materials of supercapacitors was firstly synthesized by thermally treating the graphene-bismuth composite, which was obtained through simultaneous solvothermal reduction of the colloidal dispersions of negatively charged graphene oxide sheets in N,N-dimethyl formamide (DMF) solution of bismuth cations at 180 o C. The morphology, composition, and microstructure of the composites together with pure graphite oxide, and graphene were characterized using powder X-ray diffraction (XRD), FT-IR, field emission scanning electron microscopy (FESEM), transmission electron microscope (TEM), thermogravimetry and differential thermogravimetry (TG-DTG). The electrochemical behaviors were measured by cyclic voltammogram (CV), galvanostatic charge-discharge and electrochemical impedance spectroscopy (EIS). The specific capacitance of 255 F g -1 (based on composite) is obtained at a specific current of 1 A g -1 as compared with 71 F g -1 for pure graphene. The loaded-bismuth oxide achieves a specific capacitance as high as 757 F g -1 even at 10 A g -1 . In addition, the graphene nanosheet-bismuth oxide composite electrode exhibits the excellent rate capability and well reversibility.

Facile solvothermal synthesis of a graphene nanosheet-bismuth oxide composite and its electrochemical characteristics

Energy Technology Data Exchange (ETDEWEB)

Wang Huanwen [Key Laboratory of Eco-Environment-Related Polymer Materials of Ministry of Education, Key Laboratory of Polymer Materials of Gansu Province, College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China); Hu Zhongai, E-mail: zhongai@nwnu.edu.c [Key Laboratory of Eco-Environment-Related Polymer Materials of Ministry of Education, Key Laboratory of Polymer Materials of Gansu Province, College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China); Chang Yanqin; Chen Yanli; Lei Ziqiang; Zhang Ziyu; Yang Yuying [Key Laboratory of Eco-Environment-Related Polymer Materials of Ministry of Education, Key Laboratory of Polymer Materials of Gansu Province, College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China)

2010-12-01

This work demonstrates a novel and facile route for preparing graphene-based composites comprising of metal oxide nanoparticles and graphene. A graphene nanosheet-bismuth oxide composite as electrode materials of supercapacitors was firstly synthesized by thermally treating the graphene-bismuth composite, which was obtained through simultaneous solvothermal reduction of the colloidal dispersions of negatively charged graphene oxide sheets in N,N-dimethyl formamide (DMF) solution of bismuth cations at 180 {sup o}C. The morphology, composition, and microstructure of the composites together with pure graphite oxide, and graphene were characterized using powder X-ray diffraction (XRD), FT-IR, field emission scanning electron microscopy (FESEM), transmission electron microscope (TEM), thermogravimetry and differential thermogravimetry (TG-DTG). The electrochemical behaviors were measured by cyclic voltammogram (CV), galvanostatic charge-discharge and electrochemical impedance spectroscopy (EIS). The specific capacitance of 255 F g{sup -1} (based on composite) is obtained at a specific current of 1 A g{sup -1} as compared with 71 F g{sup -1} for pure graphene. The loaded-bismuth oxide achieves a specific capacitance as high as 757 F g{sup -1} even at 10 A g{sup -1}. In addition, the graphene nanosheet-bismuth oxide composite electrode exhibits the excellent rate capability and well reversibility.

Microwave synthesis of molybdenum doped LiFePO4/C and its electrochemical studies.

Science.gov (United States)

Naik, Amol; P, Sajan C

2016-05-10

A Mo-doped LiFePO4 composite was prepared successfully from an iron carbonyl complex by adopting a facile and rapid microwave assisted solid state method. The evolution of gases from the iron precursor produces a highly porous product. The formation and substitution of Mo in LiFePO4 were confirmed by X-ray diffraction; surface analysis was carried out by scanning electron microscopy, field emission scanning electron microscopy, and transmission electron microscopy. The electrochemical properties of the substituted LiFePO4 were examined by cyclic voltammetry, electrochemical impedance spectroscopy and by recording charge-discharge cycles. It was observed that the as prepared composites consisted of a single phase orthorhombic olivine-type structure, where Mo(6+) was successfully introduced into the M2(Fe) sites. Incorporation of supervalent Mo(6+) introduced Li(+) ion vacancies in LiFePO4. The synthesized material facilitated lithium ion diffusion during charging/discharging due to the charge compensation effect and porosity. The battery performance studies showed that LiMo0.05Fe0.095PO4 exhibited a maximum capacity of 169.7 mA h g(-1) at 0.1 C current density, with admirable stability retention. Even at higher current densities, the retention of the specific capacity was exceptional.

Electrochemically deposited hybrid nickel-cobalt hexacyanoferrate nanostructures for electrochemical supercapacitors

International Nuclear Information System (INIS)

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

2011-01-01

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

Electrochemically deposited hybrid nickel-cobalt hexacyanoferrate nanostructures for electrochemical supercapacitors

Energy Technology Data Exchange (ETDEWEB)

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

2011-10-30

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

Hydrothermal synthesis and electrochemical characterization of VO2 (B) with controlled crystal structures

International Nuclear Information System (INIS)

Jiang Wentao; Ni Juan; Yu Ke; Zhu Ziqiang

2011-01-01

Three different VO 2 (B) nanostructures, including urchin-like VO 2 (B), VO 2 (B) honeycombs and VO 2 (B) nanorods have been successfully fabricated through hydrothermal process by adjusting the concentrations of the oxalic acid. The microstructure and morphology of the VO 2 nanostructures were evaluated by using X-ray diffraction and scanning and transmission electron microscopies. Electrochemical properties measurements of urchin-like VO 2 (B) and VO 2 (B) honeycombs showed excellent cycling performance, especially the urchin-like VO 2 (B) exhibited higher discharge capacity and better capacity retention.

Nano-TiO{sub 2} coatings on aluminum surfaces by aerosol flame synthesis

Energy Technology Data Exchange (ETDEWEB)

Liberini, Mariacira; De Falco, Gianluigi; Scherillo, Fabio; Astarita, Antonello [Dipartimento di Ingegneria Chimica, dei Materiali e della Produzione Industriale, Università degli Studi di Napoli Federico II, Napoli 80125 (Italy); Commodo, Mario; Minutolo, Patrizia [Istituto di Ricerche sulla Combustione, CNR, Napoli 80125 (Italy); D' Anna, Andrea, E-mail: anddanna@unina.it [Dipartimento di Ingegneria Chimica, dei Materiali e della Produzione Industriale, Università degli Studi di Napoli Federico II, Napoli 80125 (Italy); Squillace, Antonino [Dipartimento di Ingegneria Chimica, dei Materiali e della Produzione Industriale, Università degli Studi di Napoli Federico II, Napoli 80125 (Italy)

2016-06-30

Aluminum alloys are widely used in the aeronautic industry for their high mechanical properties; however, because they are very sensitive to corrosion, surface treatments are often required. TiO{sub 2} has excellent resistance to oxidation and it is often used to improve the corrosion resistance of aluminum surfaces. Several coating procedures have been proposed over the years, which are in some cases expensive in terms of production time and amount of deposited material. Moreover, they can damage aluminum alloys if thermal treatments are required. In this paper, a one-step method for the coating of aluminum surfaces with titania nanoparticles is presented. Narrowly sized, TiO{sub 2} nanoparticles are synthesized by flame aerosol and directly deposited by thermophoresis onto cold plates of aluminum AA2024. Submicron coatings of different thicknesses are obtained from two flame synthesis conditions by varying the total deposition time. A fuel-lean synthesis condition was used to produce 3.5 nm pure anatase nanoparticles, while a mixture of rutile and anatase nanoparticles having 22 nm diameter — rutile being the predominant phase —, was synthesized in a fuel-rich condition. Scanning electron microscopy is used to characterize morphology of titania films, while coating thickness is measured by confocal microscopy measurements. Electrochemical impedance spectroscopy is used to evaluate corrosion resistance of coated aluminum substrates. Results show an improvement of the electrochemical behavior of titania coated surfaces as compared to pristine aluminum surfaces. The best results are obtained by covering the substrates with 3.5 nm anatase-phase nanoparticles and with lower deposition times, that assure a uniform surface coating. - Highlights: • Nanosized TiO{sub 2} particles produced by aerosol flame synthesis • Coatings of aluminum substrates with TiO{sub 2} nanoparticles by thermophoretic deposition in flames • Thickness measurement by confocal microscopy

XPS-nanocharacterization of organic layers electrochemically grafted on the surface of SnO_2 thin films to produce a new hybrid material coating

International Nuclear Information System (INIS)

Drevet, R.; Dragoé, D.; Barthés-Labrousse, M.G.; Chaussé, A.; Andrieux, M.

2016-01-01

Graphical abstract: An innovative hybrid material layer is synthesized by combining two processes. SnO_2 thin films are deposited by MOCVD on Si substrates and an organic layer made of carboxyphenyl moieties is electrochemically grafted by the reduction of a diazonium salt. XPS characterizations are carried out to assess the efficiency of the electrochemical grafting. Display Omitted - Highlights: • An innovative hybrid material layer is synthesized by combining two processes. • SnO_2 thin films are deposited by MOCVD on Si substrates. • An organic layer is electrochemically grafted by the reduction of a diazonium salt. • The efficiency of the grafting is accurately assessed by XPS. • Three electrochemical grafting models are proposed. - Abstract: This work presents the synthesis and the characterization of hybrid material thin films obtained by the combination of two processes. The electrochemical grafting of organic layers made of carboxyphenyl moieties is carried out from the reduction of a diazonium salt on tin dioxide (SnO_2) thin films previously deposited on Si substrates by metal organic chemical vapor deposition (MOCVD). Since the MOCVD experimental parameters impact the crystal growth of the SnO_2 layer (i.e. its morphology and its texturation), various electrochemical grafting models can occur, producing different hybrid materials. In order to evidence the efficiency of the electrochemical grafting of the carboxyphenyl moieties, X-ray Photoelectron Spectroscopy (XPS) is used to characterize the first nanometers in depth of the synthesized hybrid material layer. Then three electrochemical grafting models are proposed.

Fluorinated Phosphorene: Electrochemical Synthesis, Atomistic Fluorination, and Enhanced Stability.

Science.gov (United States)

Tang, Xian; Liang, Weiyuan; Zhao, Jinlai; Li, Zhongjun; Qiu, Meng; Fan, Taojian; Luo, Crystal Shaojuan; Zhou, Ye; Li, Yu; Guo, Zhinan; Fan, Dianyuan; Zhang, Han

2017-12-01

Phosphorene has attracted great interest due to its unique electronic and optoelectronic properties owing to its tunable direct and moderate band-gap in association with high carrier mobility. However, its intrinsic instability in air seriously hinders its practical applications, and problems of technical complexity and in-process degradation exist in currently proposed stabilization strategies. A facile pathway in obtaining and stabilizing phosphorene through a one-step, ionic liquid-assisted electrochemical exfoliation and synchronous fluorination process is reported in this study. This strategy enables fluorinated phosphorene (FP) to be discovered and large-scale, highly selective few-layer FP (3-6 atomic layers) to be obtained. The synthesized FP is found to exhibit unique morphological and optical characteristics. Possible atomistic fluorination configurations of FP are revealed by core-level binding energy shift calculations in combination with spectroscopic measurements, and the results indicate that electrolyte concentration significantly modulates the fluorination configurations. Furthermore, FP is found to exhibit enhanced air stability thanks to the antioxidation and antihydration effects of the introduced fluorine adatoms, and demonstrate excellent photothermal stability during a week of air exposure. These findings pave the way toward real applications of phosphorene-based nanophotonics. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and characterization of oligobenzimidazoles: Electrochemical, electrical, optical, thermal and rectification properties

Science.gov (United States)

Anand, Siddeswaran; Muthusamy, Athianna

2018-03-01

A series of benzimidazole monomers, (2-(2, 4-dihydroxyphenyl)-1H-benzimidazol-5-yl)(phenyl) methanone (BIKH), 2-(3-ethoxy-2-hydroxyphenyl)-1H-benzo [d]imidazole-5-yl) (phenyl) methanone (BIKE) and 2-(5-bromo-2-hydroxyphenyl)-1H-benzo [d]imidazole-5-yl) (phenyl) methanone (BIKB) were prepared by condensing three substituted aromatic aldehydes with 3, 4-diaminobenzophenone. In aqueous alkaline medium the benzimidazoles were converted in to oligomers by oxidative polycondensation using NaOCl as oxidant. The formation of monomers and oligomers were confirmed with 1H, 13C NMR, FT-IR, and UV-visible spectroscopic techniques. The oligomers were investigated for their optical, electrical, electrochemical and thermal properties. The electrochemical and optical band gaps of monomers and oligomers were calculated using both UV-visible spectroscopy and cyclic voltametry respectively. The band gap values of monomers are compared with band gap values obtained from quantum theoretical calculations with DFT. The electrical conductivity studies of iodine doped and undoped oligomers were done using two point probe technique. It is found that these values are showing good correlation with the charge densities on imidazole nitrogen obtained from Huckel method. The conductivity of oligomers increases with increase in iodine vapour contact time. The dielectric properties of oligomers have been investigated at different temperature and frequency. The dielectric measurement data were used to calculate the AC conductivity and activation energy of oligomers. Oligomer OBIKH is having greater thermal stability due to its number of chain propagation sites than other oligomers and is shown by its high carbines residue of around 60% at 600 °C in thermogravimetric analysis. I-V characteristics of oligobenzimidazole p-n diodes have shown good rectifying nature in the range -4 to 4 V.

Electrochemical Sensors for Clinic Analysis

Directory of Open Access Journals (Sweden)

Guang Li

2008-03-01

Full Text Available Demanded by modern medical diagnosis, advances in microfabrication technology have led to the development of fast, sensitive and selective electrochemical sensors for clinic analysis. This review addresses the principles behind electrochemical sensor design and fabrication, and introduces recent progress in the application of electrochemical sensors to analysis of clinical chemicals such as blood gases, electrolytes, metabolites, DNA and antibodies, including basic and applied research. Miniaturized commercial electrochemical biosensors will form the basis of inexpensive and easy to use devices for acquiring chemical information to bring sophisticated analytical capabilities to the non-specialist and general public alike in the future.

Synthesis of multilayered structure of nano-dimensional silica glass/reduced graphene oxide for advanced electrochemical applications.

Science.gov (United States)

Ghosh, Arnab; Miah, Milon; Majumder, Chinmoy; Bag, Shekhar; Chakravorty, Dipankar; Saha, Shyamal Kumar

2018-03-28

During the past few years, intensive research has been carried out to design new functional materials for superior electrochemical applications. Due to low storage capacity and low charge transport, silica based glasses have not yet been investigated for their supercapacitive behavior. Therefore, in the present study, a multilayered structure of silica-based nanoglass and reduced graphene oxide has been designed to remarkably enhance the specific capacitance by exploiting the porosity, large surface area, sufficient dangling bonds in the nanoglass and high electrical conductivity of rGO. The charge transport in the composite structure is also investigated to understand the electrochemical properties. It is found that Simmons tunneling or direct tunneling is the dominant mechanism of charge conduction between the graphene layers via the potential barrier of silica nanoglass phase. We believe that this study will open up a new area in the design of glass-based two-dimensional nanocomposites for superior supercapacitor applications.

Investigation of the electrochemical deposition of thick layers of cadmium telluride

International Nuclear Information System (INIS)

Rousset, J.

2007-04-01

This research thesis deals with the problem of electrochemical deposition of thick layers of cadmium telluride (CdTe) meeting the requirements of high energy radiation detection. The author first recalls the physicochemical properties of CdTe and the basic principles of radiology. He details the different criteria which define a material for X ray detection. He describes the experimental conditions, the nature and preparation of substrates, and the different electrochemical systems used in this research. He studies the impact of the applied potential on the material properties, and compares previously obtained results available in the literature with those obtained in the chosen pool conditions. He discusses the synthesis of CdTe thick layers for which different methods are tested: static in potential, static in intensity, pulsed. The coatings obtained with a given potential and then with a given current are investigated. Finally, the influence of a thermal treatment in presence or absence of a sintering agent on the morphology, the chemical composition, and the crystalline and electric properties of the deposited material is discussed, and the results of the behaviour under X rays of a electrodeposited layer are presented

Electrochemical biosensors for hormone analyses.

Science.gov (United States)

Bahadır, Elif Burcu; Sezgintürk, Mustafa Kemal

2015-06-15

Electrochemical biosensors have a unique place in determination of hormones due to simplicity, sensitivity, portability and ease of operation. Unlike chromatographic techniques, electrochemical techniques used do not require pre-treatment. Electrochemical biosensors are based on amperometric, potentiometric, impedimetric, and conductometric principle. Amperometric technique is a commonly used one. Although electrochemical biosensors offer a great selectivity and sensitivity for early clinical analysis, the poor reproducible results, difficult regeneration steps remain primary challenges to the commercialization of these biosensors. This review summarizes electrochemical (amperometric, potentiometric, impedimetric and conductometric) biosensors for hormone detection for the first time in the literature. After a brief description of the hormones, the immobilization steps and analytical performance of these biosensors are summarized. Linear ranges, LODs, reproducibilities, regenerations of developed biosensors are compared. Future outlooks in this area are also discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

Electrochemical study of nitrobenzene reduction using novel Pt nanoparticles/macroporous carbon hybrid nanocomposites

International Nuclear Information System (INIS)

Zhang Yufan; Zeng Lijun; Bo Xiangjie; Wang Huan; Guo Liping

2012-01-01

Graphical abstract: A one-step microwave-assisted route for rapidly synthesizing Pt nanoparticles ensemble on macroporous carbon hybrid nanocomposites (PNMPC) has been reported. As a novel electrode material, the excellent electrochemical behavior of nitrobenzene was investigated thoroughly at the PNMPC modified glassy carbon electrode. And moreover, the modified electrode was successfully applied to the determination of nitrobenzene in real samples. Highlights: ► One-step microwave-assisted heating synthesis Pt nanoparticles/macroporous carbon hybrid nanocomposites (PNMPC). ► Catalytic rate constant being 3.14 × 10 4 M −1 s −1 for NB in pH 7.0. ► Sensitive electrochemical detection of NB at the PNMPC/Nafion/GC electrode. ► The electrode showing excellent anti-interference ability and good stability for NB. - Abstract: Novel Pt nanoparticles (PN) ensemble on macroporous carbon (MPC) hybrid nanocomposites (PNMPC) were prepared through a rapidly and simple one-step microwave-assisted heating procedure. The obtained PNMPC was characterized by transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA) and electrochemical methods. The electrochemical reduction of nitrobenzene (NB) was thoroughly investigated at the PNMPC modified glassy carbon (GC) electrode, and the catalytic rate constant was calculated to be 3.14 × 10 4 M −1 s −1 for NB. A sensitive NB sensor was developed based on the PNMPC/GC electrode, which showed a wide linear range (1–200 μM), low detection limit (50 nM), high sensitivity (6.93 μA μM −1 ), excellent anti-interference ability and good stability. And moreover, the electrode was successfully applied to the determination of NB in real samples.

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-03-15

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

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

International Nuclear Information System (INIS)

Park, Sumi; Kim, Kyuwon

2016-01-01

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

Synthesis of nitrogen doped microporous carbons prepared by activation-free method and their high electrochemical performance

International Nuclear Information System (INIS)

Kim, Ki-Seok; Park, Soo-Jin

2011-01-01

Graphical abstract: This describes the increase of specific capacitance in hybrid electrodes as a function of melamine content. Display Omitted Highlights: → For N-enriched hybrid carbons, co-precursors, PVDF/melamine composites, were used. → Microporous carbons were formed by only carbonization without chemical activation. → The nitrogen content of microporous carbons was controlled by melamine content. → N-doped carbons showed higher specific capacitance compared to microporous carbons. → It was attributed to the easy electron transfer and pseudocapacitance. - Abstract: Nitrogen-doped microporous carbons (N-MCs) were prepared by the carbonization of the polyvinylidene fluoride (PVDF)/melamine mixture without chemical activation. The electrochemical performance of the N-MCs was investigated as a function of PVDF/melamine ratio. It was found that, without additional activation, the N-MCs had a high specific surface area (greater than 560 m 2 /g) because of the micropore formation by the release of fluorine groups. In addition, although the specific surface area decreased, nitrogen groups were increased with increasing melamine content, leading to an enhanced electrochemical performance. Indeed, the N-MCs showed a better electrochemical performance than that of microporous carbons (MCs) prepared by PVDF alone, and the highest specific capacitance (310 F/g) was obtained at a current density of 0.5 A/g, as compared to a value of 248 F/g for MCs. These results indicate that the microporous features of N-MC lead to feasible ion transfer during charge/discharge duration and the presence of nitrogen groups as strong electron donor on the N-MC electrode in electrolyte could provide a pseudocapacitance by the redox reaction.

Energy and power performance of electrochemical double-layer capacitors based on molybdenum carbide derived carbon

International Nuclear Information System (INIS)

Thomberg, T.; Jaenes, A.; Lust, E.

2010-01-01

Cyclic voltammetry, constant current charge/discharge, and electrochemical impedance spectroscopy have been applied to establish the electrochemical characteristics for electric double-layer capacitor (EDLC) consisting of the 1 M (C 2 H 5 ) 3 CH 3 NBF 4 electrolyte in acetonitrile and micro/mesoporous carbon electrodes prepared from Mo 2 C, noted as C(Mo 2 C). The N 2 sorption (total BET specific surface area (S BET ≤ 1855 m 2 g -1 ), micropore area (S micro ≤ 1823 m 2 g -1 ), total pore volume (V tot ≤ 1.399 m 3 g -1 ) and pore size distribution (average NLDFT pore width d NLDFT ≥ 0.89 nm) values obtained have been correlated with the electrochemical characteristics for EDLCs (region of ideal polarizability (ΔV = 3.0 V), characteristic time constant (τ R = 1.05 s), gravimetric capacitance (C m ≤ 143 F g -1 )) dependent strongly on the C(Mo 2 C) synthesis temperature. High gravimetric energy (35 Wh kg -1 ) and gravimetric power (237 kW kg -1 ) values, normalised to the total active mass of both C(Mo 2 C) electrodes, synthesised at T synt = 800 deg. C, have been demonstrated at cell voltage 3.0 V and T = 20 deg. C.

A high-performance flexible fibre-shaped electrochemical capacitor based on electrochemically reduced graphene oxide.

Science.gov (United States)

Li, Yingru; Sheng, Kaixuan; Yuan, Wenjing; Shi, Gaoquan

2013-01-11

A fibre-shaped solid electrochemical capacitor based on electrochemically reduced graphene oxide has been fabricated, exhibiting high specific capacitance and rate capability, long cycling life and attractive flexibility.

XPS-nanocharacterization of organic layers electrochemically grafted on the surface of SnO{sub 2} thin films to produce a new hybrid material coating

Energy Technology Data Exchange (ETDEWEB)

Drevet, R., E-mail: richarddrevet@yahoo.fr [Univ. Paris Sud, SP2M-ICMMO, CNRS UMR 8182, Bât. 410, 91405 Orsay Cedex (France); Université d’Evry Val d’Essonne, LAMBE, CNRS-CEA UMR 8587, Boulevard François Mitterrand, 91025 Evry Cedex (France); Dragoé, D.; Barthés-Labrousse, M.G. [Univ. Paris Sud, SP2M-ICMMO, CNRS UMR 8182, Bât. 410, 91405 Orsay Cedex (France); Chaussé, A. [Université d’Evry Val d’Essonne, LAMBE, CNRS-CEA UMR 8587, Boulevard François Mitterrand, 91025 Evry Cedex (France); Andrieux, M. [Univ. Paris Sud, SP2M-ICMMO, CNRS UMR 8182, Bât. 410, 91405 Orsay Cedex (France)

2016-10-30

Graphical abstract: An innovative hybrid material layer is synthesized by combining two processes. SnO{sub 2} thin films are deposited by MOCVD on Si substrates and an organic layer made of carboxyphenyl moieties is electrochemically grafted by the reduction of a diazonium salt. XPS characterizations are carried out to assess the efficiency of the electrochemical grafting. Display Omitted - Highlights: • An innovative hybrid material layer is synthesized by combining two processes. • SnO{sub 2} thin films are deposited by MOCVD on Si substrates. • An organic layer is electrochemically grafted by the reduction of a diazonium salt. • The efficiency of the grafting is accurately assessed by XPS. • Three electrochemical grafting models are proposed. - Abstract: This work presents the synthesis and the characterization of hybrid material thin films obtained by the combination of two processes. The electrochemical grafting of organic layers made of carboxyphenyl moieties is carried out from the reduction of a diazonium salt on tin dioxide (SnO{sub 2}) thin films previously deposited on Si substrates by metal organic chemical vapor deposition (MOCVD). Since the MOCVD experimental parameters impact the crystal growth of the SnO{sub 2} layer (i.e. its morphology and its texturation), various electrochemical grafting models can occur, producing different hybrid materials. In order to evidence the efficiency of the electrochemical grafting of the carboxyphenyl moieties, X-ray Photoelectron Spectroscopy (XPS) is used to characterize the first nanometers in depth of the synthesized hybrid material layer. Then three electrochemical grafting models are proposed.

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-12-30

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

Synthesis of feather-like CeO2 microstructures and enzymatic electrochemical catalysis for trichloroacetic acid

Science.gov (United States)

Xiao, Xin; Zhang, Dong En; Zhang, Fan; Gong, Jun Yan; Zhang, Xiao Bo; Wang, Yi Hui; Ma, Juan Juan; Tong, Zhi Wei

Novel feather-like CeO2 microstructures were achieved by a thermal decomposition approach of Ce(OH)CO3 precursor. The Ce(OH)CO3 was obtained from a solvothermal method employing Ce(NO3)3.6H2O with C6H12N4 and C16H33(CH3)3NBr (CTAB) at 190∘C in a water-PEG-200 mixed solution. The feather-like CeO2 dendrite was obtained by thermal conversion of the feather-like Ce(OH)CO3 at 650∘C in air. A reasonable growth mechanism was proposed with the soft-template effect of PEG-200. The electrochemical behavior and enzyme activity of myoglobin (Mb) immobilized on CeO2-Nafion modified glassy carbon electrode (GCE) are demonstrated by cyclic voltammetric measurements. The results indicate that CeO2 can obviously promote the direct electron transfer between the Mb redox centers and the electrode. The Mb on CeO2-Nafion behaves as an elegant performance on the electrochemical reduction of trichloroacetic acid (TCA) from 0.32μM to 2.28μM. The detection limit is estimated to be 0.08μM.

GC of catalytic reactions products involved in the promising fuel synthesis

Energy Technology Data Exchange (ETDEWEB)

Zheivot, V.; Sazonova, N. [Russian Academy of Sciences, Novosibirsk (Russian Federation). Boreskov Inst. of Catalysis

2012-09-15

Catalytic reactions involved in the synthesis of the promising kinds of novel fuel and products formed in these reactions were systematized according to the resulting fuel type. Generalization of the retention of the substances comprising these products is presented. Chromatograms exhibiting their separation on chromatographic materials with the surface of different chemical properties are summarized. We propose procedures for gas-chromatographic analysis of the catalytic reactions products formed in the synthesis of hydrogen, methanol, dimethyl ether and hydrocarbons as a new generation of fuel alternative to petroleum and coal. For partial oxidation of methane into synthesis gas, on-line determination of the components obtained in the reaction was carried out by gas chromatography and gas analyzer based on different physicochemical methods (IR spectroscopy and electrochemical methods). Similarity of the results obtained using these methods is demonstrated. (orig.)

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-10-15

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

A Critical Review of Spinel Structured Iron Cobalt Oxides Based Materials for Electrochemical Energy Storage and Conversion

Directory of Open Access Journals (Sweden)

Hongyan Gao

2017-11-01

Full Text Available Iron cobalt oxides, such as typical FeCo2O4 and CoFe2O4, are two spinel structured transitional metal oxide materials with excellent electrochemical performance. As the electrodes, they have been widely applied in the current energy storage and conversion processes such as supercapacitors, Lithium-ion batteries and fuel cells. Based on synthesis approaches and controlled conditions, these two materials exhibited broad morphologies and nanostructures and thus distinct electrochemical performance. Some of them have shown promising applications as electrodes in energy storage and conversion. The incorporation with other materials to form composites further improved their performance. This review briefly summarized the recent applications of FeCo2O4 and CoFe2O4 in energy storage and conversion, current understandings on mechanisms and especially the relevance of morphologies and structures and composites to electrochemical performance. Some recommendations were finally put forward addressing current issues and future prospects on electrodes of FeCo2O4 and CoFe2O4 based materials in energy storage and conversion, implying there was still space to further optimize their performance.

Synthesis and characterization of MgO nanocrystals for biosensing applications

Energy Technology Data Exchange (ETDEWEB)

Li, Hongji [Tianjin Key Laboratory of Organic Solar Cells and Photochemical Conversion, School of Chemistry & Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China); Li, Mingji, E-mail: limingji@163.com [Tianjin Key Laboratory of Film Electronic and Communication Devices, School of Electronics Information Engineering, Tianjin University of Technology, Tianjin 300384 (China); Qiu, Guojun [Tianjin Key Laboratory of Organic Solar Cells and Photochemical Conversion, School of Chemistry & Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China); Li, Cuiping; Qu, Changqing; Yang, Baohe [Tianjin Key Laboratory of Film Electronic and Communication Devices, School of Electronics Information Engineering, Tianjin University of Technology, Tianjin 300384 (China)

2015-05-25

Highlights: • MgO nanocrystals were prepared using DC arc plasma jet CVD method. • The growth time does not exceed 10 min in process of the synthesis. • The samples were found to consist of cubic MgO nanobelts and nanosheets. • Nanocrystals contain contacts, rough edges, vacancies, and doping defects. • The samples exhibited excellent electrochemical biosensing properties. - Abstract: MgO nanocrystals were prepared using a simple direct current arc plasma jet chemical vapor deposition method. Magnesium nitrate was used as source material and Mo film was used as a substrate and catalyst. The high-temperature plasma produced ensured rapid synthesis of the MgO nanocrystals. The as-prepared nanocrystals were characterized by field-emission scanning electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction, energy-dispersive spectroscopy, Fourier transform infrared spectrometry, ultraviolet–visible spectrophotometry, and photoluminescence measurements. The as-synthesized samples were found to consist of cubic MgO nanobelts and nanosheets with large surface areas and low coordination oxide ions, and contained numerous contacts, rough edges, vacancies, and doping defects. The nanostructures exhibited excellent electrochemical sensing properties with high-sensing sensitivity toward ascorbic acid. Their high electrocatalytic activity was attributed to the effect of defects and the surface electron transfer ability of the one-dimensional MgO nanobelts.

Electrochemical Analysis of Neurotransmitters

Science.gov (United States)

Bucher, Elizabeth S.; Wightman, R. Mark

2015-07-01

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

Synthesis and electrochemical properties of ZnMn_2O_4 anode for lithium-ion batteries

International Nuclear Information System (INIS)

Feng, Chuanqi; Wang, Wei; Chen, Xiao; Wang, Shiquan; Guo, Zaiping

2015-01-01

Graphical abstract: ZnMn_2O_4 nanoparticles were prepared through the rheological phase reaction method (R-ZMO) or the mixed solvothermal method(M-ZMO). The particles of M-ZMO were clustered together to form uniform microspheres morphology. The M-ZMO behaved higher reversible capacity and better cycle performance than that of R-ZMO. - Highlights: • ZnMn_2O_4 nanoparticles were prepared through the rheological phase reaction method (R-ZMO) or the mixed solvothermal method (M-ZMO). • The M-ZMO behaved higher reversible capacity and better cycle performance than that of R-ZMO. • The morphology and cell parameters of ZnMn_2O_4 are important effects on its electrochemical properties. • The diffusion coefficient of Li"+ in M-ZMO is beneficial for M-ZMO to be used an anode. - Abstract: The precursors of ZnMn_2O_4 were synthesized by different methods (the rheological phase reaction method or the mixed solvothermal method). The precursors were heat-treated at a suitable temperature to obtain the expected product (ZnMn_2O_4). The synthesized samples were characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The electrochemical properties of the samples were also investigated. The results show that ZnMn_2O_4 was synthesized successfully. The particles of ZnMn_2O_4 were irregular quasi-spheres with sizes of about 50 nm. The ZnMn_2O_4 nanoparticles synthesized through the mixed solvothermal method were clustered together to form microspheres about 1 μm in diameter. The electrochemical testing results showed that the ZnMn_2O_4 synthesized through the mixed solvothermal method featured higher reversible capacity and better cycling performance than the sample synthesized by the rheological phase reaction method. The ZnMn_2O_4 synthesized through the mixed solvothermal method could be a promising anode material for lithium ion battery application.

Hydrothermal synthesis of electrode materials pyrochlore tungsten trioxide film

Science.gov (United States)

Guo, Jingdong; Li, Yingjeng James; Stanley Whittingham, M.

Hydrothermal synthesis methods have been successfully used to prepare new transition-metal oxides for cathodes in electrochemical devices such as lithium batteries and electrochromic windows. The tungsten oxides were the first studied, but the method has been extended to the oxides of molybdenum, vanadium and manganese. Sodium tungsten oxide films with the pyrochlore structure have been prepared on gold/alumina and indium-doped tin oxide substrates. These films reversibly and rapidly intercalate lithium and hydrogen ions.

Electrochemical oxidation of organic waste

International Nuclear Information System (INIS)

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

1990-01-01

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

Electrochemical synthesis of SnCo alloy shells on orderly rod-shaped Cu current collectors as anode materials for lithium-ion batteries with enhanced performance

Energy Technology Data Exchange (ETDEWEB)

Zhan, Fangwei; Zhang, Hui, E-mail: meszhanghui@zju.edu.cn; Qi, Yue; Wang, Jiazheng; Du, Ning; Yang, Deren

2013-09-05

Highlights: •Nanostructured SnCo/Cu electrodes have been successfully fabricated. •A simple electrodeposition approach was employed. •The Cu arrays offer large surface area and improve electronic/ionic conductivity. •The electrodes show improved performance as anode for Li-ion batteries. •The improved performance was attributed to the nanostructured current collectors. -- Abstract: In this article, we report a two-step electrodeposition method for the synthesis of Cu/SnCo core–shell rod-shaped arrays as anodes of lithium-ion batteries. Firstly, the arrayed Cu nanorods with diameters of 200 nm were fabricated on a Cu foil through an electrodeposition method with alumina oxide membrane (AAO) as the template. Secondly, the SnCo alloy shells were subsequently electrodeposited on the surface of the rod-shaped Cu arrays to form the hybrid nanostructures. These hybrid electrodes delivered the enhanced cyclic performance and high rate capability serving as the anode materials for lithium-ion batteries. The improved electrochemical performance might be attributed to the large surface-to-volume area, sufficient buffering space, and high electronic conductivity associated with these 3-dimensional (3D) nanostructures.

Ultrasensitive molecularly imprinted electrochemical sensor based on magnetism graphene oxide/β-cyclodextrin/Au nanoparticles composites for chrysoidine analysis

International Nuclear Information System (INIS)

Wang, Xiaojiao; Li, Xiangjun; Luo, Chuannan; Sun, Min; Li, Leilei; Duan, Huimin

2014-01-01

Highlights: • Synthesis and application of MGO/β-CD@AuNPs as a sensor for chrysoidine analysis. • The synthesized polymer had a laminar structure with high surface. • The propose sensor showed high selectivity and good sensitivity. - Abstract: A imprinted electrochemical sensor based on glassy carbon electrode (GCE) for ultrasensitive detection of chrysoidine was fabricated. A GCE was modified by magnetic graphene oxide/β-cyclodextrin/gold nanoparticles composites (MGO/β-CD@AuNPs). The sensing surface area and electronic transmission rate were increased, which was benefited from the distribution property of MGO/β-CD@AuNPs. The MGO/β-CD@AuNPs composite improved electrochemical response and sensitivity of the sensor. The molecularly imprinted electrochemical sensor was prepared by electropolymerization on modified electrode. Chrysoidine and pyrrole were used as template molecule and functional monomer, respectively. Under the optimization experimental conditions, the electrochemical sensor exhibited excellent analytical performance: the detection of chrysoidine ranged from 5.0 × 10 −8 mol/L to 5.0 × 10 −6 mol/L with the detection limit of 1.7 × 10 −8 mol/L. The sensor was applied to determine chrysoidine in spiked water samples and showed high selectivity, good sensitivity and acceptable reproducibility. The proposed method provides a promising platform for trace amount detection of other food additives

Electrochemically Functionalized Seamless Three-Dimensional Graphene-Carbon Nanotube Hybrid for Direct Electron Transfer of Glucose Oxidase and Bioelectrocatalysis.

Science.gov (United States)

Terse-Thakoor, Trupti; Komori, Kikuo; Ramnani, Pankaj; Lee, Ilkeun; Mulchandani, Ashok

2015-12-01

Three-dimensional seamless chemical vapor deposition (CVD) grown graphene-carbon nanotubes (G-CNT) hybrid film has been studied for its potential in achieving direct electron transfer (DET) of glucose oxidase (GOx) and its bioelectrocatalytic activity in glucose detection. A two-step CVD method was employed for the synthesis of seamless G-CNT hybrid film where CNTs are grown on already grown graphene film on copper foil using iron as a catalyst. Physical characterization using SEM and TEM show uniform dense coverage of multiwall carbon nanotubes (MWCNT) grown directly on graphene with seamless contacts. The G-CNT hybrid film was electrochemically modified to introduce oxygenated functional groups for DET favorable immobilization of GOx. Pristine and electrochemically functionalized G-CNT film was characterized by electrochemical impedance spectroscopy (EIS), cyclic voltammetry, X-ray photoelectron-spectroscopy, and Raman spectroscopy. The DET between GOx and electrochemically oxidized G-CNT electrode was studied using cyclic voltammetry which showed a pair of well-defined and quasi-reversible redox peaks with a formal potential of -459 mV at pH 7 corresponding to the redox site of GOx. The constructed electrode detected glucose concentration over the clinically relevant range of 2-8 mM with the highest sensitivity of 19.31 μA/mM/cm(2) compared to reported composite hybrid electrodes of graphene oxide and CNTs. Electrochemically functionalized CVD grown seamless G-CNT structure used in this work has potential to be used for development of artificial mediatorless redox enzyme based biosensors and biofuel cells.

Electrochemical, morphological and microstructural characterization of carbon film resistor electrodes for application in electrochemical sensors

International Nuclear Information System (INIS)

Gouveia-Caridade, Carla; Soares, David M.; Liess, Hans-Dieter; Brett, Christopher M.A.

2008-01-01

The electrochemical and microstructural properties of carbon film electrodes made from carbon film electrical resistors of 1.5, 15, 140 Ω and 2.0 kΩ nominal resistance have been investigated before and after electrochemical pre-treatment at +0.9 V vs SCE, in order to assess the potential use of these carbon film electrodes as electrochemical sensors and as substrates for sensors and biosensors. The results obtained are compared with those at electrodes made from previously investigated 2 Ω carbon film resistors. Cyclic voltammetry was performed in acetate buffer and phosphate buffer saline electrolytes and the kinetic parameters of the model redox system Fe(CN) 6 3-/4- obtained. The 1.5 Ω resistor electrodes show the best properties for sensor development with wide potential windows, similar electrochemical behaviour to those of 2 Ω and close-to-reversible kinetic parameters after electrochemical pre-treatment. The 15 and 140 Ω resistor electrodes show wide potential windows although with slower kinetics, whereas the 2.0 kΩ resistor electrodes show poor cyclic voltammetric profiles even after pre-treatment. Electrochemical impedance spectroscopy related these findings to the interfacial properties of the electrodes. Microstructural and morphological studies were carried out using contact mode Atomic Force Microscopy (AFM), Confocal Raman spectroscopy and X-ray diffraction. AFM showed more homogeneity of the films with lower nominal resistances, related to better electrochemical characteristics. X-ray diffraction and Confocal Raman spectroscopy indicate the existence of a graphitic structure in the carbon films

Enhanced Electrochemical Hydrogen Storage Performance on the Porous Graphene Network Immobilizing Cobalt Metal Nanoparticle

Energy Technology Data Exchange (ETDEWEB)

Kang, Myunggoo; Lee, Dong Heon; Jung, Hyun [Dongguk University, Seoul (Korea, Republic of)

2016-05-15

In this study, we attempted to apply Co metal nanoparticles decorated on the surface of the porous graphene (Co-PG) as the electrochemical hydrogen storage system. Co-PG was successfully synthesized by the soft-template method. To determine the synthetic strategy of porous graphene and Co nanoparticles, we compare the obtained Co-PG with two different materials such as Co nanoparticle decorated reduced graphene oxide without soft-template (Co-RGO) and porous graphene without Co nanoparticle (PG). The experimental details regarding the synthesis and characterization of the Co-PG, Co-RGO, and PG samples are provided in Supporting Information. Co-PG with interpenetrating porous networks and immobilized Co metal nanoparticles were successfully synthesized by the soft-template method. The obtained Co-PG exhibited high-surface area with ink-bottle open pores owing to the homogeneous dispersion of P123 micellar rods. The XRD and FE-SEM analyses clearly confirm that Co nanoparticles were immobilized on to the surface of porous graphene without any significant aggregation. The as-obtained Co-PG showed good electrochemical performance such as capacity and cycle stability for hydrogen storage. Based on these results, we believe that the Co-PG with a high-specific surface area could be worthwhile to investigate as not only electrochemical hydrogen storage materials but also other energy storage applications.

Enhanced Electrochemical Hydrogen Storage Performance on the Porous Graphene Network Immobilizing Cobalt Metal Nanoparticle

International Nuclear Information System (INIS)

Kang, Myunggoo; Lee, Dong Heon; Jung, Hyun

2016-01-01

In this study, we attempted to apply Co metal nanoparticles decorated on the surface of the porous graphene (Co-PG) as the electrochemical hydrogen storage system. Co-PG was successfully synthesized by the soft-template method. To determine the synthetic strategy of porous graphene and Co nanoparticles, we compare the obtained Co-PG with two different materials such as Co nanoparticle decorated reduced graphene oxide without soft-template (Co-RGO) and porous graphene without Co nanoparticle (PG). The experimental details regarding the synthesis and characterization of the Co-PG, Co-RGO, and PG samples are provided in Supporting Information. Co-PG with interpenetrating porous networks and immobilized Co metal nanoparticles were successfully synthesized by the soft-template method. The obtained Co-PG exhibited high-surface area with ink-bottle open pores owing to the homogeneous dispersion of P123 micellar rods. The XRD and FE-SEM analyses clearly confirm that Co nanoparticles were immobilized on to the surface of porous graphene without any significant aggregation. The as-obtained Co-PG showed good electrochemical performance such as capacity and cycle stability for hydrogen storage. Based on these results, we believe that the Co-PG with a high-specific surface area could be worthwhile to investigate as not only electrochemical hydrogen storage materials but also other energy storage applications

Green synthesis of cobalt (II, III) oxide nanoparticles using Moringa Oleifera natural extract as high electrochemical electrode for supercapacitors

Science.gov (United States)

Matinise, N.; Mayedwa, N.; Fuku, X. G.; Mongwaketsi, N.; Maaza, M.

2018-05-01

The research work involved the development of a better, inexpensive, reliable, easily and accurate way for the fabrication of Cobalt (II, III) oxide (Co3O4) nanoparticles through a green synthetic method using Moringa Oleifera extract. The electrochemical activity, crystalline structure, morphology, isothermal behaviour and optical properties of Co3O4 nanoparticles were studied using various characterization techniques. The X-ray diffraction (XRD) and Energy Dispersive X-ray Spectroscopy (EDS) analysis confirmed the formation of Co3O4 nanoparticles. The pseudo-capacitor behaviour of spinel Co3O4 nanoparticles on Nickel foam electrode was investigated by cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS) in 3M KOH solution. The CV curve revealed a pairs of redox peaks, indicating the pseudo-capacitive characteristics of the Ni/Co3O4 electrode. EIS results showed a small semicircle and Warburg impedance, indicating that the electrochemical process on the surface electrode is kinetically and diffusion controlled. The charge-discharge results indicating that the specific capacitance Ni/Co3O4 electrode is approximately 1060 F/g at a discharge current density of at 2 A/g.

Electrochemical behavior of high performance on-chip porous carbon films for micro-supercapacitors applications in organic electrolytes

Science.gov (United States)

Brousse, K.; Huang, P.; Pinaud, S.; Respaud, M.; Daffos, B.; Chaudret, B.; Lethien, C.; Taberna, P. L.; Simon, P.

2016-10-01

Carbide derived carbons (CDCs) are promising materials for preparing integrated micro-supercapacitors, as on-chip CDC films are prepared via a process fully compatible with current silicon-based device technology. These films show good adherence on the substrate and high capacitance thanks to their unique nanoporous structure which can be fine-tuned by adjusting the synthesis parameters during chlorination of the metallic carbide precursor. The carbon porosity is mostly related to the synthesis temperature whereas the thickness of the films depends on the chlorination duration. Increasing the pore size allows the adsorption of large solvated ions from organic electrolytes and leads to higher energy densities. Here, we investigated the electrochemical behavior and performance of on-chip TiC-CDC in ionic liquid solvent mixtures of 1-ethyl-3-methylimidazolium tetrafluoroborate (EMIBF4) diluted in either acetonitrile or propylene carbonate via cyclic voltammetry and electrochemical impedance spectroscopy. Thin CDC films exhibited typical capacitive signature and achieved 169 F cm-3 in both electrolytes; 65% of the capacitance was still delivered at 1 V s-1. While increasing the thickness of the films, EMI+ transport limitation was observed in more viscous PC-based electrolyte. Nevertheless, the energy density reached 90 μW h cm-2 in 2M EMIBF4/ACN, confirming the interest of these CDC films for micro-supercapacitors applications.

Synthesis and electrochemical properties of spinel Li(Li{sub 0.05}Cu{sub 0.05}Mn{sub 1.90})O{sub 4} by a flameless combustion method

Energy Technology Data Exchange (ETDEWEB)

Hao, Jiabin; Bai, Hongli; Liu, Jintao; Yang, Fangli; Li, Qiling; Su, Changwei [Key Laboratory of Comprehensive Utilization of Mineral Resources in Ethnic Regions, Yunnan Minzu University, Kunming 650500 (China); Key Laboratory of Resource Clean Conversion in Ethnic Regions, Education Department of Yunnan, Yunnan Minzu University, Kunming 650500 (China); Engineering Research Center of Biopolymer Functional Materials of Yunnan, Yunnan Minzu University, Kunming 650500 (China); Guo, Junming, E-mail: guojunming@tsinghua.org.cn [Key Laboratory of Comprehensive Utilization of Mineral Resources in Ethnic Regions, Yunnan Minzu University, Kunming 650500 (China); Key Laboratory of Resource Clean Conversion in Ethnic Regions, Education Department of Yunnan, Yunnan Minzu University, Kunming 650500 (China); Engineering Research Center of Biopolymer Functional Materials of Yunnan, Yunnan Minzu University, Kunming 650500 (China)

2016-05-25

A (Li, Cu)-co-doped cathode material Li(Li{sub 0.05}Cu{sub 0.05}Mn{sub 1.90})O{sub 4} was prepared by a flameless combustion synthesis at 500 °C for 3 h and then two-stage calcination at 700 °C for 6 h. Physical and electrochemical performances were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscope (TEM), galvanostatic charge–discharge cycling test, cyclic voltammogram (CV) and electrochemical impedance spectroscopy (EIS) to investigate the influence of Li and Cu substitution on the lithium ion batteries. Li(Li{sub 0.05}Cu{sub 0.05}Mn{sub 1.90})O{sub 4} not only exhibited the initial discharge capacity of 106.9 mAh g{sup −1} with a high retention of 89.2% after 500 cycles at 1.0 C but also retained 63.5% capacity after 1500 cycles at 5.0 C. Besides, a good rate capability at different current densities from 0.5 C to 5.0 C can be acquired. The (Li, Cu)-co-doped sample had excellent cycling stability in comparison with the LiMn{sub 2}O{sub 4} cathode. - Highlights: • A (Li, Cu)-co-doped Li(Li{sub 0.05}Cu{sub 0.05}Mn{sub 1.90})O{sub 4} was synthesized by a flameless combustion method. • The (Li, Cu)-co-doped Li(Li{sub 0.05}Cu{sub 0.05}Mn{sub 1.90})O{sub 4} has higher crystallinity. • Low level of Li and Cu doping exhibits better rate capability and cycling performance.

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

International Nuclear Information System (INIS)

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

2008-01-01

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

Nanostructured inorganic materials: Synthesis and associated electrochemical properties

Science.gov (United States)

Yau, Shali Zhu

Synthetic strategy for preparing potential battery materials at low temperature was developed. Magnetite (Fe3O4), silver hollandnite (AgxMn8O16), magnesium manganese oxide (MgxMnO 2˙yH2O), and silver vanadium phosphorous oxide (Ag 2VO2PO4) were studied. Magnetite (Fe3O4) was prepared by coprecipitation induced by triethylamine from aqueous iron(II) and iron(III) chloride solutions of varying concentrations. Variation of the iron(II) and iron(III) concentrations results in crystallite size control of the Fe3O4 products. Materials characterization of the Fe3O4 samples is reported, including Brunauer-Emmitt-Teller (BET) surface area, x-ray powder diffraction (XRD), transmission electron microscopy (TEM), particle size, and saturation magnetization results. A strong correlation between discharge capacity and voltage recovery behavior versus crystallite size was observed when tested as an electrode material in lithium electrochemical cells. Silver hollandite (AgxMn8O16) was successfully synthesized through a low temperature reflux reaction. The crystallite size and silver content of AgxMn8O16 by varying the reactant ratio of silver permanganate (AgMnO4) and manganese sulfate monohydrate (MnSO4˙H2O). Silver hollandite was characterized by Brunauer-Emmitt-Teller (BET) surface area, inductively coupled plasma-optical emission (ICP-OES) spectrometry, helium pycnometry, simultaneous thermogravimetric analysis/differential scanning calorimetry (TGA/DSC), and x-ray powder diffraction (XRD). The crystallite size showed a strong correlation with silver content, BET surface area, and particle sizes. The silver hollandite cathode showed good discharge capacity retention in 30 cycles of discharge-charge. There were a good relationship between crystallite size and rate capability and pulse ability. Magnesium manganese oxide (MgxMnO2˙yH 2O) was made by redox reaction by mixing sodium hydroxide (NaOH), manganese sulfate monohydrate (MnSO4˙HO2), and potassium persulfate (K2S2O8

A novel solution combustion synthesis of cobalt oxide nanoparticles as negative-electrode materials for lithium ion batteries

International Nuclear Information System (INIS)

Wen Wei; Wu Jinming; Tu Jiangping

2012-01-01

Highlights: ► We examine the electrochemical performance of cobalt oxides fabricated by solution combustion synthesis for rechargeable lithium-ion battery applications. ► The additive of NaF in precursor results in an eruption combustion mode. ► The eruption combustion leads to fluffy networks with smaller grains and more macroporous voids. ► The network contributes to higher discharge capacity, higher initial coulombic efficiency, and better cycling performance for rechargeable lithium-ion batteries. - Abstract: Low cost mass production of cobalt oxide nanoparticles with high electrochemical performance is of practical interest for rechargeable lithium-ion batteries. In this report, cobalt oxide nanoparticles were fabricated by solution combustion synthesis, with the introduction of NaF into the precursor to alter the combustion mode. The novel eruption combustion resulted in fluffy networks with smaller particles and more macroporous voids, which contributed to the higher discharge capacity, higher initial coulombic efficiency, and better cycling performance when compared with that achieved by the conventional combustion mode.

Large-scale synthesis of ultrathin Au-Pt nanowires assembled on thionine/graphene with high conductivity and sensitivity for electrochemical immunosensor

International Nuclear Information System (INIS)

Lu, Wenbo; Ge, Juan; Tao, Lin; Cao, Xiaowei; Dong, Jian; Qian, Weiping

2014-01-01

In this article, for the first time, a novel, label-free and inherent electroactive redox biosensor based on ultrathin Au-Pt nanowire-decorated thionine/reduced graphene oxide (AuPtNWs/THI/rGO) is developed for carcinoembryonic antigen (CEA) detection. Ultrathin AuPtNWs are prepared by a one-pot synthesis method without the use of any stabilizer or template. The AuPtNWs/THI/rGO composites are obtained by the THI/rGO composites surface functionalized with -NH 2 group employed as a support for loading ultrathin AuPtNWs by coordination. The AuPtNWs/THI/rGO composites not only favor the immobilization of antibody but also facilitate the electron transfer. It is found that the resultant AuPtNWs/THI/rGO composites can be designed to act as a sensitive label-free electrochemical immunosensor for CEA determination. Under the optimized conditions, the linear range of the proposed immunosensor is estimated to be from 50 fg·mL −1 to 100 ng·mL −1 (R= 0.998) and the detection limit is estimated to be 6 fg·mL −1 at a signal-to-noise ratio of 3, respectively. The prepared immunosensor for detection of CEA shows high sensitivity, reproducibility and stability. Our study demonstrates that the proposed immunosensor has also been used to determine CEA successfully in diluted blood samples

Facile and green synthesis of mesoporous Co3O4 nanocubes and their applications for supercapacitors

Science.gov (United States)

Liu, Xiangmei; Long, Qing; Jiang, Chunhui; Zhan, Beibei; Li, Chen; Liu, Shujuan; Zhao, Qiang; Huang, Wei; Dong, Xiaochen

2013-06-01

Nanostructured Co3O4 materials attracted significant attention due to their exceptional electrochemical (pseudo-capacitive) properties. However, rigorous preparation conditions are needed to control the size (especially nanosize), morphology and size distribution of the products obtained by conventional methods. Herein, we describe a novel one step shape-controlled synthesis of uniform Co3O4 nanocubes with a size of 50 nm with the existence of mesoporous carbon nanorods (meso-CNRs). In this synthesis process, meso-CNRs not only act as a heat receiver to directly obtain Co3O4 eliminating the high-temperature post-calcination, but also control the morphology of the resulting Co3O4 to form nanocubes with uniform distribution. More strikingly, mesoporous Co3O4 nanocubes are obtained by further thermal treatment. The structure and morphology of the samples were characterized by scanning electron microscopy, transmission electron microscopy and X-ray diffraction. A possible formation mechanism of mesoporous Co3O4 nanocubes is proposed here. Electrochemical tests have revealed that the prepared mesoporous Co3O4 nanocubes demonstrate a remarkable performance in supercapacitor applications due to the porous structure, which endows fast ion and electron transfer.Nanostructured Co3O4 materials attracted significant attention due to their exceptional electrochemical (pseudo-capacitive) properties. However, rigorous preparation conditions are needed to control the size (especially nanosize), morphology and size distribution of the products obtained by conventional methods. Herein, we describe a novel one step shape-controlled synthesis of uniform Co3O4 nanocubes with a size of 50 nm with the existence of mesoporous carbon nanorods (meso-CNRs). In this synthesis process, meso-CNRs not only act as a heat receiver to directly obtain Co3O4 eliminating the high-temperature post-calcination, but also control the morphology of the resulting Co3O4 to form nanocubes with uniform

One-step synthesis of redox-active polymer/AU nanocomposites for electrochemical immunoassay of multiplexed tumor markers.

Science.gov (United States)

Liu, Zhimin; Rong, Qinfeng; Ma, Zhanfang; Han, Hongliang

2015-03-15

In this work, a simple and sensitive multiplexed immunoassay protocol for simultaneous electrochemical determination of alpha-fetoprotein (AFP) and carcinoembryonic antigen (CEA) was designed using redox-active nanocomposites. As the redox-active species, the poly(o-phenylenediamine) (POPD)/Au nanocomposite and poly(vinyl ferrocene-2-aminothiophenol) (poly(VFc-ATP))/Au nanocomposite were obtained by one-step method which HAuCl4 was used as the oxidant. With Au nanoparticles (AuNPs), the nanocomposites were successful to immobilize labeled anti-CEA and anti-AFP as the immunosensing probes. The proposed electrochemical immunoassay enabled the simultaneous monitoring of AFP and CEA in a wide range of 0.01-100ngmL(-1). The detection limits was 0.006ngmL(-1) for CEA and 0.003ngmL(-1) for AFP (S/N=3). The assay results of serum samples with the proposed method were well consistent with the reference values from standard ELISA method. And the negligible cross-reactivity between the two analytes makes it possesses potential promise in clinical diagnosis. Copyright © 2014 Elsevier B.V. All rights reserved.

Three-Dimensional ZnO Hierarchical Nanostructures: Solution Phase Synthesis and Applications

Directory of Open Access Journals (Sweden)

Xiaoliang Wang

2017-11-01

Full Text Available Zinc oxide (ZnO nanostructures have been studied extensively in the past 20 years due to their novel electronic, photonic, mechanical and electrochemical properties. Recently, more attention has been paid to assemble nanoscale building blocks into three-dimensional (3D complex hierarchical structures, which not only inherit the excellent properties of the single building blocks but also provide potential applications in the bottom-up fabrication of functional devices. This review article focuses on 3D ZnO hierarchical nanostructures, and summarizes major advances in the solution phase synthesis, applications in environment, and electrical/electrochemical devices. We present the principles and growth mechanisms of ZnO nanostructures via different solution methods, with an emphasis on rational control of the morphology and assembly. We then discuss the applications of 3D ZnO hierarchical nanostructures in photocatalysis, field emission, electrochemical sensor, and lithium ion batteries. Throughout the discussion, the relationship between the device performance and the microstructures of 3D ZnO hierarchical nanostructures will be highlighted. This review concludes with a personal perspective on the current challenges and future research.

Synthesis of ZnO micro-pompons by soft template-directed wet chemical method and their application in electrochemical biosensors

International Nuclear Information System (INIS)

Zhou, Yu; Wang, Lei; Ye, Zhizhen; Zhao, Minggang; Huang, Jingyun

2014-01-01

Highlights: •ZnO micro-pompons (MPs) are synthesized by a controlled soft template-directed route. •ZnO MPs are composed of radial robust nanowires built of numerous nanoparticles. •The structure is ideal for the immobilization of enzymes to maintain their activity. •ZnO MPs are favorable for electron transfer and liquid mobilization. •Good performance of H 2 O 2 biosensor indicates ZnO MPs are promising in biosensing. -- Abstract: ZnO micro-pompons are fabricated by a controlled synthesis route via a soft template-directed wet chemical method followed by a subsequent calcination in air. The achieved ZnO micro-pompons with several hundred micrometers in diameter are composed of a great number of robust nanowires built of numerous nanoparticles. This unique structure is accessible for enzymes to sequester or bind, and the tightly connected nanoparticles facilitate the transmission of electrons, what's more, the large spaces between the nanowires are favorable for the mobilization of the liquid with target substance. In addition, the high electron communication features of ZnO and the tightly connected nanoparticles of the structure also promote the electron transfer between the active sites of proteins and the electrode. The enzymatic electrode fabricated with Horseradish peroxidase immobilized on ZnO micro-pompons along with chitosan covering outside exhibits excellent response for detecting H 2 O 2 with a wide linear range of 0.2–3.4 mM and a high sensitivity of 1395.64 (μA/mM cm 2 ), indicating a great potential in fabricating electrochemical biosensors

Solvothermal synthesis and electrochemical performance of Li2MnSiO4/C cathode materials for lithium ion batteries

International Nuclear Information System (INIS)

Wang, Yan-Chao; Zhao, Shi-Xi; Zhai, Peng-Yuan; Li, Fang; Nan, Ce-Wen

2014-01-01

Highlights: • Li 2 MnSiO 4 /C nanocomposite has been synthesized by the solvothermal method. • The particles of Li 2 MnSiO 4 /C are much smaller and more uniform. • The presence of Ni improves discharge capacity of Li 2 MnSiO 4 /C cathode material. • The initial discharge capacity of Ni-modified Li 2 MnSiO 4 /C is 274.5 mAh g −1 at 25 °C. - Abstract: Orthorhombic structure Li 2 MnSiO 4 /C with Pmn2 1 space group is synthesized by the solvothermal method. Carbon coating and Ni 2+ doping are used to improve the electronic conductivity and the cycling performance of Li 2 MnSiO 4 cathode material, respectively. The particles of Li 2 MnSiO 4 /C are much smaller and more uniform than those of Li 2 MnSiO 4 due to the carbon coating. It is shown that Ni 2+ has been reduced into metal Ni during the synthesis process. The synthesized Ni-modified Li 2 MnSiO 4 /C (denoted as (LMS@Ni)/C) cathode material exhibits better electrochemical performance in comparison with Li 2 MnSiO 4 /C, attributing to higher lithium ion diffusion coefficient as well as electronic conductivity. The initial discharge capacity of (LMS@Ni)/C is 274.5 mA h g −1 and the reversible capacity after 20 cycles is 119.8 mA h g −1 at 25 °C

First examples of organosilica-based ionogels: synthesis and electrochemical behavior

Directory of Open Access Journals (Sweden)

Andreas Taubert

2017-03-01

Full Text Available The article describes the synthesis and properties of new ionogels for ion transport. A new preparation process using an organic linker, bis(3-(trimethoxysilylpropylamine (BTMSPA, yields stable organosilica matrix materials. The second ionogel component, the ionic liquid 1-methyl-3-(4-sulfobutylimidazolium 4-methylbenzenesulfonate, [BmimSO3H][PTS], can easily be prepared with near-quantitative yields. [BmimSO3H][PTS] is the proton conducting species in the ionogel. By combining the stable organosilica matrix with the sulfonated ionic liquid, mechanically stable, and highly conductive ionogels with application potential in sensors or fuel cells can be prepared.

Electrochemical gating in scanning electrochemical microscopy

NARCIS (Netherlands)

Ahonen, P.; Ruiz, V.; Kontturi, K.; Liljeroth, P.; Quinn, B.M.

2008-01-01

We demonstrate that scanning electrochemical microscopy (SECM) can be used to determine the conductivity of nanoparticle assemblies as a function of assembly potential. In contrast to conventional electron transport measurements, this method is unique in that electrical connection to the film is not

Nanostructured Metal Oxide Coatings for Electrochemical Energy Conversion and Storage Electrodes

Science.gov (United States)

Cordova, Isvar Abraxas

The realization of an energy future based on safe, clean, sustainable, and economically viable technologies is one of the grand challenges facing modern society. Electrochemical energy technologies underpin the potential success of this effort to divert energy sources away from fossil fuels, whether one considers alternative energy conversion strategies through photoelectrochemical (PEC) production of chemical fuels or fuel cells run with sustainable hydrogen, or energy storage strategies, such as in batteries and supercapacitors. This dissertation builds on recent advances in nanomaterials design, synthesis, and characterization to develop novel electrodes that can electrochemically convert and store energy. Chapter 2 of this dissertation focuses on refining the properties of TiO2-based PEC water-splitting photoanodes used for the direct electrochemical conversion of solar energy into hydrogen fuel. The approach utilized atomic layer deposition (ALD); a growth process uniquely suited for the conformal and uniform deposition of thin films with angstrom-level thickness precision. ALD's thickness control enabled a better understanding of how the effects of nitrogen doping via NH3 annealing treatments, used to reduce TiO2's bandgap, can have a strong dependence on TiO2's thickness and crystalline quality. In addition, it was found that some of the negative effects on the PEC performance typically associated with N-doped TiO2 could be mitigated if the NH 3-annealing was directly preceded by an air-annealing step, especially for ultrathin (i.e., transparent electrode based on a network of solution-processed Cu/Ni cores/shell nanowires (NWs) were activated by electrochemically converting the Ni metal shell into Ni(OH)2. Furthermore, an adjustment of the molar percentage of Ni plated onto the Cu NWs was found to result in a tradeoff between capacitance, transmittance, and stability of the resulting nickel hydroxide-based electrode. The nominal area capacitance and power

Structural and electrochemical analysis of chemically synthesized microcubic architectured lead selenide thin films

Science.gov (United States)

Bhat, T. S.; Shinde, A. V.; Devan, R. S.; Teli, A. M.; Ma, Y. R.; Kim, J. H.; Patil, P. S.

2018-01-01

The present work deals with the synthesis of lead selenide (PbSe) thin films by simple and cost-effective chemical bath deposition method with variation in deposition time. The structural, morphological, and electrochemical properties of as-deposited thin films were examined using characterization techniques such as X-ray diffraction spectroscopy (XRD), field-emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), galvanostatic charge-discharge and electrochemical impedance spectroscopy. XRD reveals formation of rock salt phase cubic structured PbSe. FE-SEM images show the formation of microcubic structured morphology. The existence of the PbSe is confirmed from the XPS analysis. On the other hand, CV curves show four reaction peaks corresponding to oxidation [PbSe and Pb(OH)2] and reduction (PbO2 and Pb(OH)2) at the surface of PbSe thin films. The PbSe:2 sample deposited for 80 min. shows maximum specific capacitance of 454 ± 5 F g- 1 obtained at 0.25 mA cm- 2 current density. The maximum energy density of 69 Wh kg- 1 was showed by PbSe:2 electrode with a power density of 1077 W kg- 1. Furthermore, electrochemical impedance studies of PbSe:2 thin film show 80 ± 3% cycling stability even after 500 CV cycles. Such results show the importance of microcubic structured PbSe thin film as an anode in supercapacitor devices.

Effect of symbiotic compound Fe{sub 2}P{sub 2}O{sub 7} on electrochemical performance of LiFePO{sub 4}/C cathode materials

Energy Technology Data Exchange (ETDEWEB)

Liu, Shuxin, E-mail: liushuxin88@126.com [School of Chemistry and Chemical Engineering, Mianyang Normal University, Mianyang, Sichuan 621000 (China); Gu, Chunlei [School of Chemical and Pharmaceutical Engineering, Hebei University of Science and Technology, Shijiazhuang, Hebei 050018 (China); Wang, Haibin [School of Chemistry and Chemical Engineering, Mianyang Normal University, Mianyang, Sichuan 621000 (China); Liu, Ruijiang [School of Pharmacy, Jiangsu University, Zhenjiang, Jiangsu 212013 (China); Wang, Hong; He, Jichuan [School of Chemistry and Chemical Engineering, Mianyang Normal University, Mianyang, Sichuan 621000 (China)

2015-10-15

In order to study the effect of symbiotic compound Fe{sub 2}P{sub 2}O{sub 7} on electrochemical performance of LiFePO{sub 4}/C cathode materials, the LiFePO{sub 4}/Fe{sub 2}P{sub 2}O{sub 7}/C cathode materials were synthesized by in-situ synthesis method. The phase compositions and microstructures of the products were characterized by X-ray powder diffraction (XRD) and field emission scanning electron microscope (FESEM). Results indicate that the existence of Fe{sub 2}P{sub 2}O{sub 7} does not alter LiFePO{sub 4} crystal structure and the existence of Fe{sub 2}P{sub 2}O{sub 7} decreases the particles size of LiFePO{sub 4}. The electrochemical behavior of cathode materials was analyzed using galvanostatic measurement and cyclic voltammetry (CV). The results show that the existence of Fe{sub 2}P{sub 2}O{sub 7} improves electrochemical performance of LiFePO{sub 4} cathode materials in specific capability and lithium ion diffusion rate. The charge–discharge specific capacity and apparent lithium ion diffusion coefficient increase with Fe{sub 2}P{sub 2}O{sub 7} content and maximizes around the Fe{sub 2}P{sub 2}O{sub 7} content is 5 wt%. It has been had further proved that the Fe{sub 2}P{sub 2}O{sub 7} adding enhances the lithium ion transport to improve the electrochemical performance of LiFePO{sub 4} cathode materials. However, excessive Fe{sub 2}P{sub 2}O{sub 7} will block the electron transfer pathway and affect the electrochemical performances of LiFePO{sub 4} directly. - Graphical abstract: The LiFePO{sub 4}/Fe{sub 2}P{sub 2}O{sub 7}/C cathode materials were synthesized by in-situ synthesis method. The existence of Fe{sub 2}P{sub 2}O{sub 7} does not alter LiFePO{sub 4} crystal structure and the existence of Fe{sub 2}P{sub 2}O{sub 7} decreases the particles size of LiFePO{sub 4}. The charge–discharge specific capacity and apparent lithium ion diffusion coefficient increase with Fe{sub 2}P{sub 2}O{sub 7} content. However, excessive Fe{sub 2}P{sub 2}O{sub 7} will

Recent advances in synthesis of three-dimensional porous graphene and its applications in construction of electrochemical (bio)sensors for small biomolecules detection.

Science.gov (United States)

Lu, Lu

2018-07-01

Electrochemical (bio)sensors have attracted much attention due to their high sensitivity, fast response time, biocompatibility, low cost and easy miniaturization. Specially, ever-growing necessity and interest have given rise to the fast development of electrochemical (bio)sensors for the detection of small biomolecules. They play enormous roles in the life processes with various biological function, such as life signal transmission, genetic expression and metabolism. Moreover, their amount in body can be used as an indicator for diagnosis of many diseases. For example, an abnormal concentration of blood glucose can indicate hyperglycemia or hypoglycemia. Graphene (GR) shows great applications in electrochemical (bio)sensors. Compared with two-dimensional (2D) GR that is inclined to stack together due to the strong π-π interaction, monolithic 3D porous GR has larger specific area, superior mechanical strength, better stability, higher conductivity and electrocatalytic activity. So they attracted more and increasing attention as sensing materials for small biomolecules. This review focuses on the recent advances and strategies in the fabrication methods of 3D porous GR and the development of various electrochemical (bio)sensors based on porous GR and its nanocomposites for the detection of small biomolecules. The challenges and future efforts direction of high-performance electrochemical (bio)sensors based on 3D porous GR for more sensitive analysis of small biomolecules are discussed and proposed. It will give readers an overall understanding of their progress and provide some theoretical guidelines for their future efforts and development. Copyright © 2018 Elsevier B.V. All rights reserved.

Conducting polymer nanostructures: template synthesis and applications in energy storage.

Science.gov (United States)

Pan, Lijia; Qiu, Hao; Dou, Chunmeng; Li, Yun; Pu, Lin; Xu, Jianbin; Shi, Yi

2010-07-02

Conducting polymer nanostructures have received increasing attention in both fundamental research and various application fields in recent decades. Compared with bulk conducting polymers, conducting polymer nanostructures are expected to display improved performance in energy storage because of the unique properties arising from their nanoscaled size: high electrical conductivity, large surface area, short path lengths for the transport of ions, and high electrochemical activity. Template methods are emerging for a sort of facile, efficient, and highly controllable synthesis of conducting polymer nanostructures. This paper reviews template synthesis routes for conducting polymer nanostructures, including soft and hard template methods, as well as its mechanisms. The application of conducting polymer mesostructures in energy storage devices, such as supercapacitors and rechargeable batteries, are discussed.

Conducting Polymer Nanostructures: Template Synthesis and Applications in Energy Storage

Directory of Open Access Journals (Sweden)

Lijia Pan

2010-07-01

Full Text Available Conducting polymer nanostructures have received increasing attention in both fundamental research and various application fields in recent decades. Compared with bulk conducting polymers, conducting polymer nanostructures are expected to display improved performance in energy storage because of the unique properties arising from their nanoscaled size: high electrical conductivity, large surface area, short path lengths for the transport of ions, and high electrochemical activity. Template methods are emerging for a sort of facile, efficient, and highly controllable synthesis of conducting polymer nanostructures. This paper reviews template synthesis routes for conducting polymer nanostructures, including soft and hard template methods, as well as its mechanisms. The application of conducting polymer mesostructures in energy storage devices, such as supercapacitors and rechargeable batteries, are discussed.

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

Energy Technology Data Exchange (ETDEWEB)

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

2011-05-15

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

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

International Nuclear Information System (INIS)