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Sample records for semicarbazone synthesis electrochemical

  1. Synthesis and evaluation of 4-substituted semicarbazones of levulinic acid for anticonvulsant activity

    Science.gov (United States)

    Aggarwal, Navneet; Mishra, Pradeep

    2005-01-01

    Objective: A series of 4-aryl substituted semicarbazones of levulinic acid (4-oxo pentanoic acid) was designed and synthesized to meet the structural requirements essential for anticonvulsant activity. Methods: All the compounds were evaluated for anticonvulsant activity. Anticonvulsant activity was determined after intraperitoneal (i.p.) administration to mice by maximal electroshock (MES) and subcutaneous metrazol (ScMet) induced seizure methods and minimal motor impairment was determined by rotorod test. Results: A majority of the compounds exhibited significant anticonvulsant activity after intraperitoneal administration. In the present study 4-(4′-fluoro phenyl) levulinic acid semicarbazone emerged as the most active molecule, showing broad spectrum of activity with low neurotoxicity. Unsubstituted levulinic acid semicarbazone was found to be inactive in all the screens. Conclusion: The results obtained validate the hypothesis that presence of an aryl group near the semicarbazone moiety is essential for anticonvulsant activity. The results also indicate that the hydrophilic-hydrophobic site can accommodate hydrophilic groups. PMID:15973761

  2. Synthesis, Characterization and Antimicrobial Evaluation of some Thiazole-Derived Carbamates, Semicarbazones, Amides and Carboxamide

    International Nuclear Information System (INIS)

    Balawi, N.A.A.; ALShaikh, M.A.A.; Alafeefy, A.M.; Khan, K.M.

    2016-01-01

    This study comprises the synthesis and characterization of twenty thiazole-derived carbamates (3a-e), N-substituted amides (8a-h) and carboxamide (10) from 2-aminothiazoles (1a, b) via nucleophilic substitution reactions with activated carbonyl compounds including, chloroformates (2a-d), acid chlorides (7a-e) and glutaric anhydride (9), respectively. Sequential hydrazinolysis of carbamate (3e) and condensation with a variety of aldehydes and ketones (5a d) afforded the corresponding semicarbazones (6a-d). Some selected synthesized compounds were subjected to in vitro antimicrobial evaluation against common pathogens including, Gram+ve bacteria Bacillus subtilis (NRRL B-543) and Staphylococcus aureus, Gram-ve bacteria Escherichia coli (NRRLB-21), yeasts-Candida albicans (NRRLY-477) and Saccharomyces cercvisiae (NRRL Y-567) and fungs Asperigillus niger (NRRL 599). Screening results revealed that most of the tested compounds possess good antimicrobial activity compared to standard drugs. The highest inhibitory effects against Gram-ve Escherichia coli, Gram+ve Staphylococcus aureus, yeast Candida albicans and fungus Aspergillus niger was displayed by amide (8g) bearing the thiophene moiety. (author)

  3. 14-Membered cyclic bis-semicarbazones: Stereoselective synthesis and structural features

    Science.gov (United States)

    Shutalev, Anatoly D.; Fesenko, Anastasia A.; Yankov, Alexander N.; Tafeenko, Victor A.; Chernyshev, Vladimir V.

    2017-12-01

    Stereoselectivity of acid-catalyzed cyclization of 4-(1-aryl-3-oxobutyl)semicarbazide hydrazones into mixtures of trans- and cis-isomers of 14-membered cyclic bis-semicarbazones has been studied. The isomer ratio is dependent on solvent, catalyst acidity, substrate structure and concentration, reaction temperature and time, catalyst loading. The experimental data show that the macrocyclization of acyclic precursors initially formed from two molecules of substrates proceeds with low diastereoselectivity to give mixtures of trans- and cis-macrocycles followed by slow transformation of cis-isomers into trans-isomers via ring opening by a retro-aza-Michael reaction resulting in high trans-selectivity. The driving force of this isomerization is shown to be a lower solubility of trans-isomers compared with cis-isomers. Some mechanistical aspects of the macrocycle formation were confirmed by calculations performed at the DFT B3LYP/6-311++G(d,p) level of theory. Molecular structure of the obtained hexaaza macrocycles was established using single crystal and powder X-ray diffraction, IR, UV-Vis, 1H and 13C NMR spectroscopy, and DFT calculations.

  4. Two coordination polymers based on semicarbazone Schiff base and azide: synthesis, crystal structure, electrochemistry, magnetic properties and biological activity

    Czech Academy of Sciences Publication Activity Database

    Shaabani, B.; Khandar, A.A.; Dušek, Michal; Pojarová, Michaela; Mahmoudi, F.; Feher, A.; Kajňaková, M.

    2013-01-01

    Roč. 66, č. 5 (2013), s. 748-762 ISSN 0095-8972 Grant - others:AV ČR(CZ) AP0701 Program:Akademická prémie - Praemium Academiae Institutional support: RVO:68378271 Keywords : Schiff bases * semicarbazone * coordination polymer * structure analyses Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.224, year: 2013

  5. Template synthesis of two new supramolecular zinc(II) complexes containing pentadentate N.sub.3./sub.O.sub.2./sub. semicarbazone ligand: Nanostructure synthesis, Hirshfeld surface analysis, and DFT studies

    Czech Academy of Sciences Publication Activity Database

    Tyula, Y.A.; Zabardasti, A.; Goudarziafshar, H.; Roudsari, M.S.; Dušek, Michal; Eigner, Václav

    2017-01-01

    Roč. 1150, Dec (2017), s. 383-394 ISSN 0022-2860 R&D Projects: GA ČR(CZ) GA14-03276S Institutional support: RVO:68378271 Keywords : sonochemical synthesis * Hirshfeld surface analysis * DFT calculations * bis(semicarbazone) * pentagonal-bipyramidal Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 1.753, year: 2016

  6. Synthesis, spectral and thermal studies of some dioxouranium(VI) coordination compounds of 4[N -( 4- hydroxy -3- methoxybenzalidene ) amino] antipyrine semicarbazone and 4[N-(3,4,5- trimethoxybenzalidene) amino] antipyrine semicarbazone

    International Nuclear Information System (INIS)

    Singh, Lakshman; Singh, U.P.; Chakraborti, Indranil

    2001-01-01

    In view of high coordination compounds formed by actinide metal ions, the present work describes the 8, 9 and 10-coordinated compounds of dioxouranium(IV) with 4[N-(4-hydroxy-3-methoxy-benzalidene) amino] antipyrine semicarbazone (HMBAAPS) and 4[N-(3,4,5-trimethoxybenzalidene) amino] antipyrine semicarbazone (TMBAAPS) with the general composition UO 2 X 2 .L (X = Br - , I - , NCS - or ClO 4 ) and UO 2 X 2 .L (X = NO 3 - or CH 3 COO - , and L HMBAAPS or TMBAAPS). All these complexes were characterized through elemental, spectral and thermal studies. (author)

  7. Ni(II, Pd(II and Pt(II complexes with ligand containing thiosemicarbazone and semicarbazone moiety: synthesis, characterization and biological investigation

    Directory of Open Access Journals (Sweden)

    SULEKH CHANDRA

    2008-07-01

    Full Text Available The synthesis of nickel(II, palladium(II and platinum(II complexes with thiosemicarbazone and semicarbazone of p-tolualdehyde are reported. All the new compounds were characterized by elemental analysis, molar conductance measurements, magnetic susceptibility measurements, mass, 1H-NMR, IR and electronic spectral studies. Based on the molar conductance measurements in DMSO, the complexes may be formulated as [Ni(L2Cl2] and [M(L2]Cl2 (where M = Pd(II and Pt(II due to their non-electrolytic and 1:2 electrolytic nature, respectively. The spectral data are consistent with an octahedral geometry around Ni(II and a square planar geometry for Pd(II and Pt(II, in which the ligands act as bidentate chelating agents, coordinated through the nitrogen and sulphur/oxygen atoms. The ligands and their metal complexes were screened in vitro against fungal species Alternaria alternata, Aspergillus niger and Fusarium odum, using the food poison technique.

  8. Synthesis and antimicrobial activity of N1-(3-chloro-4-fluorophenyl-N4-substituted semicarbazone derivatives

    Directory of Open Access Journals (Sweden)

    Mohamed Jawed Ahsan

    2016-09-01

    Full Text Available A series of 16 N1-(3-chloro-4-fluorophenyl-N4-substituted semicarbazone derivatives were synthesized and subjected to computational pharmacokinetic studies to predict molecular properties. All the title compounds (4a–p followed the Lipinski “Rule of Five”. The synthesized compounds were characterized by elemental analyses and spectral data and the compounds (4a–p were evaluated for antimicrobial activities. Among them the compound 2-(4-hydroxybenzylidene-N-(3-chloro-4-fluorolphenylhydrazinecarboxamide (4f was found to be the most active compound that showed good antibacterial activity while the compound 2-(4-methoxybenzylidene-N-(3-chloro-4-fluorolphenylhydrazinecarboxamide (4g was moderately active against fungal strains. We have noticed that the compounds, (4f, 4k and 4d bearing OH and NO2 groups on the phenyl ring at position 4 exhibited good antibacterial activity while compound (4g bearing OCH3 on the phenyl ring at position 4 exhibited moderate antifungal activity.

  9. Template synthesis of two new supramolecular zinc(II) complexes containing pentadentate N3O2 semicarbazone ligand: Nanostructure synthesis, Hirshfeld surface analysis, and DFT studies

    Science.gov (United States)

    Tyula, Yunes Abbasi; Zabardasti, Abedien; Goudarziafshar, Hamid; Roudsari, Majid Sadeghi; Dusek, Michal; Eigner, Vaclav

    2017-12-01

    Two new zinc(II) complexes, [Zn(H2dapsc) (CH3OH)2][ZnBr2Cl2] (1) and [Zn(H2dapsc) (CH3OH)Br]Br.(CH3OH) (2), where H2dapsc is 2,6-diacetylpyridine bis(semicarbazone), were synthesized using a template method in which the pentadentate N3O2 semicarbazone ligand derived from [1 + 2] condensation of 2,6-diacetylpyridine and semicarbazide in the presence of zinc(II) ion as template agent. These compounds were characterized by IR spectroscopy, elemental analysis, and single-crystal X-ray diffraction. Their single crystal X-ray structures showed that in both complex cations, the metal center has a distorted pentagonal-bipyramidal geometry in which the semicarbazone (H2dapsc) ligand occupies the equatorial plane, while the axial positions occupy by two methanol ligands in (1) and two bromo and methanol ligands in (2). Furthermore, the impact of the close intermolecular contacts on the crystal packing of (1) and (2) have been further studied using Hirshfeld surface analysis. Density Functional Theory (DFT) method was applied for the calculation of HOMO-LUMO energy gap, atomic charges and vibrational frequencies of title complexes. Moreover, the nanostructure of zinc complex was synthesized by a sonochemical method and characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), FT-IR spectroscopy, and elemental analysis.

  10. (E-1-Phenylethanone semicarbazone

    Directory of Open Access Journals (Sweden)

    Hoong-Kun Fun

    2009-08-01

    Full Text Available In the title compound, C9H11N3O, the benzene ring is disordered over two positions with refined occupancies of 0.922 (5 and 0.078 (5. The program PLATON [Spek (2009. Acta Cryst. D65, 148–155] recommends the solution in the space group C2/m with a = 7.3050 (3, b = 6.6745 (2, c = 18.3853 (6 Å and β = 96.986 (2°. However, the large number of non-extinct reflections needed to be ignored if C2/m is chosen suggested that the space group is incorrect, even though the R values are lower than that for P21/c. The semicarbazone group is essentially planar, with a maximum deviation of 0.046 (1 Å for one of the N atoms. The mean plane of the semicarbazone group forms dihedral angles of 33.61 (8 and 39.1 (9° with the benzene ring of the major and minor components, respectively. In the crystal structure, molecules are linked by intermolecular N—H...O hydrogen bonds into extended chains along the c axis. The crystal structure is further stabilized by weak intermolucular C—H...π interactions.

  11. Electrochemical synthesis of multisegmented nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Kok, Kuan-Ying; Ng, Inn-Khuan; Saidin, Nur Ubaidah [Malaysian Nuclear Agency, Bangi, 43000 Kajang (Malaysia)

    2012-11-27

    Electrochemical deposition has emerged as a promising route for nanostructure fabrication in recent years due to the many inherent advantages it possesses. This study focuses on the synthesis of high-aspect-ratio multisegmented Au/Ni nanowires using template-directed sequential electrochemical deposition techniques. By selectively removing the Ni segments in the nanowires, high-yield of pure gold nanorods of predetermined lengths was obtained. Alternatively, the sacrificial Ni segments in the nanowires can be galvanically displaced with Bi and Te to form barbells structures with Bi{sub x}Te{sub y} nanotubes attached to neighbouring gold segments. Detailed studies on the nanostructures obtained were carried out using various microscopy, diffraction and probebased techniques for structural, morphological and chemical characterizations.

  12. The electrochemical synthesis of europium boride

    Directory of Open Access Journals (Sweden)

    Bukatova G.A.

    2003-01-01

    Full Text Available The electroreduction of boron, europium and the electrochemical synthesis of europium boride have been investigated in NaCl-KCl-NaF(10 wt. % melt on silver and molybdenum electrodes. The parameters of boron reduction in the chloride-fluoride melt have been obtained and the character of its joint deposition with europium has been studied.

  13. Hydrothermal synthesis and electrochemical properties of a ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 128; Issue 5. Hydrothermal synthesis and electrochemical properties of a coordination polymer based on dinuclear (Pyrazinyl tetrazolate) Copper(II) cations and βOctamolybdate Anions. SHAOBIN LI LI ZHANG HUIYUAN MA HAIJUN PANG. Regular Article Volume ...

  14. Synthesis, characterization and electrochemical performance of ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 40; Issue 6. Synthesis, characterization and electrochemical performance of Li 2 Ni x Fe 1 − x SiO 4 cathode materials for lithium ion batteries. A Y SHENOUDA M M S SANAD. Volume 40 Issue 6 October 2017 pp 1055-1060 ...

  15. Controlled synthesis and electrochemical properties of vanadium ...

    Indian Academy of Sciences (India)

    Vanadium oxides; nanostructured materials; chemical synthesis; electrochemical property; VO2(M). 1. Introduction. In the past decade, much attention has been paid on low dimensional nanomaterials with novel morphologies includ- ing nanobelts, nanotubes, nanowires, nanosheets, etc. They exhibit specific physical and ...

  16. Synthesis and electrochemical studies of phenylazo substituted ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 112; Issue 6. Synthesis and electrochemical studies of phenylazo substituted tetraaza macrocyclic complexes of Ni(II). Randhir Singh Suresh Kumar Amarendra Bhattacharya. Inorganic and Analytical Volume 112 Issue 6 December 2000 pp 601-605 ...

  17. Synthesis and electrochemical studies of phenylazo substituted ...

    Indian Academy of Sciences (India)

    Unknown

    Abstract. Synthesis and characterization of some phenyl azo substituted tetraaza macrocyclic complexes of Ni(II) are reported. Electrochemical behaviour of these macrocyclic complexes has been examined using polarographic, voltammetric and spectroscopic techniques. These studies show that both the ligand and the ...

  18. Synthesis, spectroscopic (FT-IR, FT-Raman, UV and NMR) and computational studies on 3t-pentyl-2r,6c-diphenylpiperidin-4-one semicarbazone.

    Science.gov (United States)

    Arockia doss, M; Savithiri, S; Rajarajan, G; Thanikachalam, V; Saleem, H

    2015-09-05

    The structural and spectroscopic studies of 3t-pentyl-2r,6c-diphenylpiperidin-4-one semicarbazone (PDPOSC) were made by adopting B3LYP/HF levels theory using 6-311++G(d,p) basis set. The FT-IR and Raman spectra were recorded in solid phase, the fundamental vibrations were assigned on the basis of the total energy distribution (TED) of the vibrational modes, calculated with scaled quantum mechanics (SQM) method and PQS program. DFT method indicates that B3LYP is superior to HF method for molecular vibrational analysis. UV-vis spectrum of the compound was recorded in different solvents in the region of 200-800 nm and the electronic properties such as excitation energies, oscillator strength, wavelengths, HOMO and LUMO energies were evaluated by time-dependent DFT (TD-DFT) approach. The polarizability and first order hyperpolarizability of the title molecule were calculated and interpreted. The hyperconjugative interaction energy (E((2))) and electron densities of donor (i) and acceptor (j) bonds were calculated using NBO analysis. In addition, MEP and atomic charges of carbon, nitrogen and oxygen were calculated using B3LYP/6-311++G(d,p) level theory. Moreover, thermodynamic properties of the title compound were calculated by B3LYP/HF, levels using 6-311++G(d,p) basis set. The (1)H and (13)C nuclear magnetic resonance (NMR) chemical shifts of the molecule were calculated by the gauge independent atomic orbital (GIAO) method and compared with experimental results. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. 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

  20. Carbon Onions: Synthesis and Electrochemical Applications

    Energy Technology Data Exchange (ETDEWEB)

    McDonough, John K. [Drexel Univ., Philadelphia, PA (United States). Dept. of Materials Science and Engineering; Gogotsi, Y. [Drexel Univ., Philadelphia, PA (United States). Dept. of Materials Science and Engineering

    2013-01-01

    Onion-like carbon structures have been synthesized in many ways and large scale production is currently under study. The annealing method can satisfy the need for large scale production, though the ideal spherical shape is unachievable, and the temperature attainable in this method is not sufficient for treating the entire particle. The arc-discharge method provides an alternate pathway toward large scale synthesis. Due to its structure and electrochemical properties, carbon onions can be used as materials for electrochemical double layer capacitors (EDLC) and can be used to store energy across a much wider temperature range, which gives these materials advantages over conventional EDLCs. This and other aspects of carbon onions are discussed in this article.

  1. 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

  2. Electrochemical synthesis and characterization of copper (I) oxide

    OpenAIRE

    Bugarinović Sanja J.; Grekulović Vesna J.; Rajčić-Vujasinović Mirjana M.; Stević Zoran M.; Stanković Zvonimir D.

    2009-01-01

    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 cupr...

  3. Electrochemical synthesis and characterization of chloride doped ...

    Indian Academy of Sciences (India)

    Unknown

    (HCl) by potentiodynamic method in an electrochemical cell and studied by cyclic voltammetry and FTIR techniques. The FTIR spectra confirmed Cl– ion doping in the ... were not hygroscopic whereas chloride doped polyaniline films were found to be highly hygroscopic. Keywords. Conducting polymer; electrochemical ...

  4. Electrochemical synthesis of alkyl nitroaromatic compounds.

    Science.gov (United States)

    Gallardo, Iluminada; Guirado, Gonzalo; Marquet, Jordi

    2003-01-24

    Alkyl nitroaromatic compounds were readily prepared via nucleophilic aromatic substitution for hydrogen or a heteroatom by electrochemical oxidation of the sigma-complex. Butyllithium and butylmagnesium chloride were used as nucleophiles, and several nitrocompounds were tested to explore the possibilities of the NASH and NASX reactions promoted electrochemically.

  5. Spectroscopic studies on Isatin-3-Semicarbazone and Isatin-3 ...

    African Journals Online (AJOL)

    ... bombardment (FAB) and negative ion chemical ionization (NICI) mass spectra are also reported. Fragmentation of molecular and pseudomolecular ions are tabulated and rationalized. KEY WORDS: IH NMR, 13C NMR, Semicarbazone thiosemicarbazone, mass spectra, negative ion chemical ionization, fragmentation.

  6. Synthesis, characterization and electrochemical performance of ...

    Indian Academy of Sciences (India)

    Scanning electron microscopy andFourier transform infrared spectroscopy investigations were carried out, which reveal the morphology and function groupsof the synthesized samples. Furthermore, electrochemical impedance spectra measurements are performed. The obtainedresults indicated that the highest conductivity ...

  7. Synthesis, characterization, X-ray crystal structure, electrochemical ...

    Indian Academy of Sciences (India)

    DOI 10.1007/s12039-015-0978-8. Synthesis, characterization, X-ray crystal structure, electrochemical evaluation and anti-cancer studies of a mixed ligand Cu(II) complex of (E)-N -((2-hydroxynaphthalen-1-yl)methylene)acetohydrazide. IRAN SHEIKHSHOAIEa, S YOUSEF EBRAHIMIPOURa,∗, MAHDIEH SHEIKHSHOAIEa,.

  8. Synthesis, spectroscopic, electrochemical and luminescence studies ...

    Indian Academy of Sciences (India)

    hydrazino-5-mercapto-1,2,4-triazole (LH2) as co-ligand were synthesised and characterized by elemental analysis, IR, UV/Vis, 1H NMR spectra and FAB-mass data. The electrochemical and luminescent properties of the complexes were also ...

  9. 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)

  10. Electrochemical Synthesis of Ammonia in Solid Electrolyte Cells

    Directory of Open Access Journals (Sweden)

    Ioannis eGaragounis

    2014-01-01

    Full Text Available Developed in the early 1900's, the Haber-Bosch synthesis is the dominant NH3 synthesis process. Parallel to catalyst optimization, current research efforts are also focused on the investigation of new methods for ammonia synthesis, including the electrochemical synthesis with the use of solid electrolyte cells. Since the first report on Solid State Ammonia Synthesis (SSAS, more than 30 solid electrolyte materials were tested and at least 15 catalysts were used as working electrodes. Thus far, the highest rate of ammonia formation reported is 1.13×10−8 mol s−1 cm−2, obtained at 80°C with a Nafion solid electrolyte and a mixed oxide, SmFe0.7Cu0.1Ni0.2O3, cathode. At high temperatures (>500oC the maximum rate was 9.5*10-9 mol s−1 cm−2 using Ce0.8Y0.2O2-δ -[Ca3(PO42 -K3PO4] as electrolyte and Ag-Pd as cathode. In this paper, the advantages and the disadvantages of SSAS vs the conventional process and the requirements that must be met in order to promote the electrochemical process into an industrial level, are discussed.

  11. Electrochemical Synthesis of Ammonia in Solid Electrolyte Cells

    International Nuclear Information System (INIS)

    Garagounis, Ioannis; Kyriakou, Vasileios; Skodra, Aglaia; Vasileiou, Eirini; Stoukides, Michael

    2014-01-01

    Developed in the early 1900s, the “Haber–Bosch” synthesis is the dominant NH 3 synthesis process. Parallel to catalyst optimization, current research efforts are also focused on the investigation of new methods for ammonia synthesis, including the electrochemical synthesis with the use of solid electrolyte cells. Since the first report on Solid State Ammonia Synthesis (SSAS), more than 30 solid electrolyte materials were tested and at least 15 catalysts were used as working electrodes. Thus far, the highest rate of ammonia formation reported is 1.13 × 10 -8 mol s -1 cm -2 , obtained at 80°C with a Nafion solid electrolyte and a mixed oxide, SmFe 0.7 Cu 0.1 Ni 0.2 O 3 , cathode. At high temperatures (>500°C), the maximum rate was 9.5 × 10 −9 mol s -1 cm -2 using Ce 0.8 Y 0.2 O 2-δ –[Ca 3 (PO 4 ) 2 –K 3 PO 4 ] as electrolyte and Ag–Pd as cathode. In this paper, the advantages and the disadvantages of SSAS vs. the conventional process and the requirements that must be met in order to promote the electrochemical process into an industrial level are discussed.

  12. 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.

  13. 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.

  14. Electrochemical synthesis and optical properties of organically capped silver nanoparticles

    International Nuclear Information System (INIS)

    Rabinal, M.K.; Kalasad, M.N.; Praveenkumar, K.; Bharadi, V.R.; Bhikshavartimath, A.M.

    2013-01-01

    Graphical abstract: A simple electrochemical method for the synthesis of organically capped silver nanoparticles by anodic dissolution of silver. Highlights: ► Electrochemical method has been developed to synthesize silver nanoparticles. ► The bulk silver is converted to monodispersed silver nanoparticles by anodic dissolution of metal. ► It permits in-situ capping of nanoparticles with suitable organic molecules. ► The method is simple, economical and greener in approach to prepare bulk quantity of stable sols of silver nanoparticles. -- Abstract: A top to bottom approach has been adopted to prepare silver nanoparticles by electrochemical dissolution of metal in suitable organic solvents. The method is being simple and economical, also permits in situ capping of nanoparticles with organic molecules. Thioglycolic acid is used as capping/stabilizing agent. Optical absorption, transmission electron microscopy, fourier transform infrared spectroscopy and X-ray diffraction measurements were carried out to study the effect of capping molecules on the size and shape of nanoparticles. It is found that thioglycolic acid is an effective capping agent and hence the resultant sol, even with high density of nanoparticles, is kinetically more stable. The present method can also be extended to synthesize other metal nanoparticles capped with various organic molecules

  15. Investigation of electrochemical synthesis of ferrate - Part II: Optimization of the process parameters of ferrate(VI electrochemical synthesis

    Directory of Open Access Journals (Sweden)

    Čekerevac Milan I.

    2010-01-01

    Full Text Available In part I [1] of the investigation the behavior of iron and selected low carbon steels in concentrated (10M - 15 M water solution of NaOH and KOH in wide range of electrode potentials, between hydrogen evolution reaction and oxygen evolution reaction, is investigated and discussed. On the base of experimental data obtained by LSV and galvanostatic pulse methods, it is concluded [1] that efficient synthesis of ferrate (VI can be expected in the region of anodic potentials between + 0,55 V and + 0,75 V against Hg|HgO reference electrode. In this paper optimization of electrolysis parameters of the electrochemical synthesis of ferrate(VI is elaborated. The most important parameters chosen for optimization process were: anode material, alkaline electrolyte concentration, regime of electrical potential control, current density and electrolyte temperature. The best current efficiency and yield of ferrate(VI synthesis of the explored anode materials (electrical steel, low carbon cold rolled steel plate, and structural steel is obtained when electrical steel with 3 wt% of silicon is applied. The worst current efficiency is obtained with anodes made of structural steel with higher concentration of manganese, chromium and nickel. The influence of alloying elements on the process of electrochemical synthesis of ferrate(VI is discussed in terms of their influence on formation and stability of anodic passive layer and oxygen evolution reaction. The increase of electrolyte concentration from 10M to 15M NaOH and KOH provided the increase of current efficiency with maximum obtained for 14M NaOH. The yield of ferrate(VI synthesis increases with temperature raise, having maximal value at about +50°C, and after that, at higher temperatures, instability of ferrate(VI increases and the yield of synthesis lessens. Considering the influence of electrical regime control it is concluded that the biggest yield of ferrate(VI can be expected with constant anodic potential

  16. 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.

  17. Electrolytes and Electrodes for Electrochemical Synthesis of Ammonia

    DEFF Research Database (Denmark)

    Lapina, Alberto

    to evaluate their applicability to electrochemical synthesis of ammonia. First a number of potential electrolytes are investigated in the temperature range 25-400°C in order to find a proton conductor with a conductivity higher than 10-4 S/cm in dry atmosphere (pH2O conductivity of materials...... 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...... 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...

  18. 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

  19. 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...

  20. 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.

  1. 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%.

  2. Lithium iron silicate sol–gel synthesis and electrochemical investigation

    Energy Technology Data Exchange (ETDEWEB)

    Oghbaei, Morteza; Baniasadi, Fazel; Asgari, Sirous, E-mail: sirousasgari@gmail.com

    2016-07-05

    Li{sub 2}FeSiO{sub 4} was synthesized through Sol–Gel method and the effect of calcination temperature, time and chelating agent concentration were investigated. Appropriate calcination temperature above 550 °C was determined by TG/DTA analysis. Afterward, the dried gel powder was calcined at each temperature of 650 °C, 700 °C and 750 °C for 1, 2 and 3 h. XRD studies illustrated the most appropriate calcination temperature of 700 °C for 1 h. To compare the effect of chelating agent concentration, citric acid with molar ratio of 1/3, 2/3 and 1 were used which 1/3 was determined as the best concentration. FE-SEM observation showed that mean grain is size lower than 100 nm. By using this material, a three electrodes test cell was assembled and its electrochemical properties were investigated. The results showed high charge capacity which could be achieved at current density of 0.05 C. - Highlights: • Sol–Gel synthesis of Li{sub 2}FeSiO{sub 4} with tetraethyl orthosilicate, lithium acetate, and iron nitrate. • The most appropriate temperature and time for calcinations were 700 °C and 1 h, respectively. • Maximum charge capacity of 175 mAh/g in Charge–discharge tests for the battery with Li{sub 2}FeSiO{sub 4} cathode. • Charge–discharge current density of C/20 for the synthesized material.

  3. 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.

  4. 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%.

  5. 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.

  6. 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

  7. 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

  8. Synthesis and reducing power assay of methyl semicarbazone derivatives

    Directory of Open Access Journals (Sweden)

    Manmohan Singhal

    2014-04-01

    Full Text Available In the present study we have designed a new pharmacophore ‘Chalconesemicarbazone’ by pharmacophore hybridization approach of drug design. A series of novel chalconesemicarbazones was synthesized and evaluated for their antioxidant activity by reducing power assay. Most of the compounds were found to be potent antioxidants. Free radicals play an important role in various pathological and xenotoxic effects so antioxidant may have protective role in these pathological conditions. Based on the results of reducing power assay 1-[1-(2,4-dihydroxyphenyl-3-(2-hydroxyphenylallylidene]-4-(4-methylphenylsemicarbazide (compound 18 and 1-[1-(2,5-dihydroxyphenyl-3-(6-hydroxyphenylallylidene]-4-(4-methylphenylsemicarbazide (compound 21 were the most active lead compounds. It was found that methoxy and hydroxyl substituted chalconesemicarbazones exhibited potent reducing power and unsubstituted compound showed less reducing potential.

  9. Experimental and theoretical studies on electrochemical synthesis of poly(3-amino-1,2,4-triazole)

    Energy Technology Data Exchange (ETDEWEB)

    Mert, Basak Dogru, E-mail: bdogru@cu.edu.tr [Cukurova University, Science and Letters Faculty, Chemistry Department, 01330 Balcal Latin-Small-Letter-Dotless-I , Adana (Turkey); Mert, M. Erman; Kardas, Guelfeza; Yaz Latin-Small-Letter-Dotless-I c Latin-Small-Letter-Dotless-I , Birguel [Cukurova University, Science and Letters Faculty, Chemistry Department, 01330 Balcal Latin-Small-Letter-Dotless-I , Adana (Turkey)

    2012-10-01

    Highlights: Black-Right-Pointing-Pointer The poly(3-amino-1,2,4-triazole) was electrochemically synthesized. Black-Right-Pointing-Pointer The homogeneous, colorful polymer has higher thermal and electrochemical stability. Black-Right-Pointing-Pointer The correlation was observed between experimental and theoretical data. - Abstract: The electrochemical synthesis of poly(3-amino-1,2,4-triazole) (PATA) on the platinum (Pt) electrode was achieved in ammonium oxalate solution by cyclic voltammetry technique. The conductivity of film was measured with four probe technique, the surface morphology was monitored with atomic force microscopy (AFM) and characterization was achieved by Fourier transform infrared spectroscopy (FT-IR) and UV-vis spectroscopy techniques. The thermal stability of polymer has also been investigated by the means of thermogravimetric analysis (TGA). The electrochemical stability of Pt/PATA was investigated in different buffer solutions. The quantum theoretical calculations employed and some parameters (dipole moment, E{sub HOMO}, E{sub LUMO}) were determined.

  10. 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

  11. Synthesis and characterization of electrochemically-reduced graphene

    Indian Academy of Sciences (India)

    Abstract. 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 ...

  12. Bio-electrochemical synthesis of commodity chemicals by ...

    Indian Academy of Sciences (India)

    electrochemical cell at −400 mV by aDC power supply at 37°C, pH 6.8, and was studied for both batch and continuous systems. Pre-enrichment ofbio-cathode enhanced the electroactivity of cells and resulted in maximizing extracellular products in ...

  13. 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 ...

  14. Synthesis, structure and spectral and electrochemical properties of ...

    Indian Academy of Sciences (India)

    Administrator

    Electrochemical measurements on the complexes in MeCN solution reveal that the lower redox potential of Ru(II)/Ru(III) couple in 4 and 6, compared to 3 and 5 respectively, is due to the enhanced s-donor capacity of benzimidazole nitrogen atoms in. 4 and 6, which leads to an increase in negative charge on ruthenium; this ...

  15. Electrochemical Synthesis of Polypyrrole Layers Doped with Glutamic Ions

    NARCIS (Netherlands)

    Meteleva-Fischer, Yulia V.; Von Hauff, Elizabeth; Parisi, Juergen

    2009-01-01

    Electrochemically synthesized polypyrrole thin films doped with glutamic ions were investigated as interesting materials for potential use as molecularly selective surfaces. Pyrrole and glutamate interact in aqueous solution, resulting in the formation of a prominent band at 240 nm in the absorption

  16. 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.

  17. 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.

  18. Direct synthesis of lithium-intercalated graphene for electrochemical energy storage application.

    Science.gov (United States)

    Kumar, Ashavani; Reddy, Arava Leela Mohana; Mukherjee, Arnab; Dubey, Madan; Zhan, Xiaobo; Singh, Neelam; Ci, Lijie; Billups, W Edward; Nagurny, John; Mital, Gandhi; Ajayan, Pulickel M

    2011-06-28

    A novel approach for bulk synthesis of lithium-intercalated graphene sheets through the reduction of exfoliated graphene oxide in liquid ammonia and lithium metal is reported. It is demonstrated here that as-synthesized lithiated graphite oxide sheets (Li-RGO) can be directly used as an electrode material in lithium batteries. The electrochemical studies on Li-RGO electrodes show a significant enhancement in the specific capacity of the lithium battery over commercially available graphite electrodes. Partial intercalation of lithium ions in between graphene layers makes this material a good candidate for electrochemical energy storage applications.

  19. 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

  20. 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.

  1. 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)

  2. 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.

  3. Synthesis and electrochemical performance of hierarchical nano-vanadium oxide.

    Science.gov (United States)

    Mjejri, I; Sediri, F

    2016-10-15

    Hierarchically structured nano-vanadium oxides with different morphologies have been synthesized via a template-free hydrothermal route by adjusting the organic precursor quantities. The effects of molar ratio on structure, morphology and crystallite sized were investigated. The possible growth mechanism is also proposed. When evaluated as a cathode material for lithium-ion batteries, the vanadium oxyhydroxide H2V3O8 samples deliver very high charging capacity, good reversibility and a better cycling stability. The excellent electrochemical performance is attributed to multiple advantageous structural features. Copyright © 2016 Elsevier Inc. All rights reserved.

  4. 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.

  5. The antimicrobial activity of lapachol and its thiosemicarbazone and semicarbazone derivatives.

    Science.gov (United States)

    Souza, Marina Azevêdo; Johann, Susana; Lima, Luciana Alves Rodrigues dos Santos; Campos, Fernanda Fraga; Mendes, Isolda Castro; Beraldo, Heloisa; Souza-Fagundes, Elaine Maria de; Cisalpino, Patrícia Silva; Rosa, Carlos Augusto; Alves, Tânia Maria de Almeida; de Sá, Nívea Pereira; Zani, Carlos Leomar

    2013-05-01

    Lapachol was chemically modified to obtain its thiosemicarbazone and semicarbazone derivatives. These compounds were tested for antimicrobial activity against several bacteria and fungi by the broth microdilution method. The thiosemicarbazone and semicarbazone derivatives of lapachol exhibited antimicrobial activity against the bacteria Enterococcus faecalis and Staphylococcus aureus with minimal inhibitory concentrations (MICs) of 0.05 and 0.10 µmol/mL, respectively. The thiosemicarbazone and semicarbazone derivatives were also active against the pathogenic yeast Cryptococcus gattii (MICs of 0.10 and 0.20 µmol/mL, respectively). In addition, the lapachol thiosemicarbazone derivative was active against 11 clinical isolates of Paracoccidioides brasiliensis, with MICs ranging from 0.01-0.10 µmol/mL. The lapachol-derived thiosemicarbazone was not cytotoxic to normal cells at the concentrations that were active against fungi and bacteria. We synthesised, for the first time, thiosemicarbazone and semicarbazone derivatives of lapachol. The MICs for the lapachol-derived thiosemicarbazone against S. aureus, E. faecalis, C. gattii and several isolates of P. brasiliensis indicated that this compound has the potential to be developed into novel drugs to treat infections caused these microbes.

  6. The antimicrobial activity of lapachol and its thiosemicarbazone and semicarbazone derivatives

    Directory of Open Access Journals (Sweden)

    Marina Azevedo Souza

    2013-05-01

    Full Text Available Lapachol was chemically modified to obtain its thiosemicarbazone and semicarbazone derivatives. These compounds were tested for antimicrobial activity against several bacteria and fungi by the broth microdilution method. The thiosemicarbazone and semicarbazone derivatives of lapachol exhibited antimicrobial activity against the bacteria Enterococcus faecalis and Staphylococcus aureus with minimal inhibitory concentrations (MICs of 0.05 and 0.10 µmol/mL, respectively. The thiosemicarbazone and semicarbazone derivatives were also active against the pathogenic yeast Cryptococcus gattii (MICs of 0.10 and 0.20 µmol/mL, respectively. In addition, the lapachol thiosemicarbazone derivative was active against 11 clinical isolates of Paracoccidioides brasiliensis, with MICs ranging from 0.01-0.10 µmol/mL. The lapachol-derived thiosemicarbazone was not cytotoxic to normal cells at the concentrations that were active against fungi and bacteria. We synthesised, for the first time, thiosemicarbazone and semicarbazone derivatives of lapachol. The MICs for the lapachol-derived thiosemicarbazone against S. aureus, E. faecalis, C. gattii and several isolates of P. brasiliensis indicated that this compound has the potential to be developed into novel drugs to treat infections caused these microbes.

  7. Agarwal N Synthesis, photophysical and electrochemical proper-ties ...

    Indian Academy of Sciences (India)

    Administrator

    A solid-polymer-electrolyte direct methanol fuel cell. (DMFC) with Pt–Ru nanoparticles supported onto poly(3,4-ethylenedioxythiophene) and polystyrene sulphonic acid polymer composite as anode. 381. Silva M M S see Dutra R F. 911. Singh A see Venugopalan P. 739. Singh A P see Gupta R. 311. Singh D. Synthesis and ...

  8. 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...

  9. Synthesis, characterization and electrochemical studies of LiNi0⋅ 8 ...

    Indian Academy of Sciences (India)

    Synthesis, characterization and electrochemical studies of LiNi0.8M0.2O2 cathode material for rechargeable lithium batteries ... Abstract. LiNiO2 and substituted nickel oxides, LiNi0.8M0.2O2 and LiCo0.8M0.2O2 (M = Mg2+, Ca2+, Ba2+), have been synthesized using simple solid state technique and used as cathode active ...

  10. Electrochemical synthesis of selenium nanotubes by using CTAB soft-template

    International Nuclear Information System (INIS)

    Zhang Shengyi; Zhang Juan; Liu Yi; Ma Xiang; Chen Hongyuan

    2005-01-01

    The single-crystalline Se nanotubes were synthesized on the surface of Au sheet electrode by cyclic voltammetry. In synthesis process, cetyltrimethyl ammonium bromide (CTAB) was used as soft-template. The formation mechanism of Se nanotubes was discussed. Furthermore, the deposits with other morphologies were also obtained by modulating parameters in the synthesis process. The products as-prepared were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and laser Raman spectrograph (LRS). The electrochemical behavior of the Se nanotubes was studied by the linear scan voltammetry

  11. 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.

  12. 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.

  13. 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)

  14. 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.

  15. Amorphous Li2 O2 : Chemical Synthesis and Electrochemical Properties.

    Science.gov (United States)

    Zhang, Yelong; Cui, Qinghua; Zhang, Xinmin; McKee, William C; Xu, Ye; Ling, Shigang; Li, Hong; Zhong, Guiming; Yang, Yong; Peng, Zhangquan

    2016-08-26

    When aprotic Li-O2 batteries discharge, the product phase formed in the cathode often contains two different morphologies, that is, crystalline and amorphous Li2 O2 . The morphology of Li2 O2 impacts strongly on the electrochemical performance of Li-O2 cells in terms of energy efficiency and rate capability. Crystalline Li2 O2 is readily available and its properties have been studied in depth for Li-O2 batteries. However, little is known about the amorphous Li2 O2 because of its rarity in high purity. Herein, amorphous Li2 O2 has been synthesized by a rapid reaction of tetramethylammonium superoxide and LiClO4 in solution, and its amorphous nature has been confirmed by a range of techniques. Compared with its crystalline siblings, amorphous Li2 O2 demonstrates enhanced charge-transport properties and increased electro-oxidation kinetics, manifesting itself a desirable discharge phase for high-performance Li-O2 batteries. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. 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.

  17. 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

  18. Electrochemical synthesis and characterization of zinc oxalate nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Shamsipur, Mojtaba, E-mail: mshamsipur@yahoo.com [Department of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Roushani, Mahmoud [Department of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Department of Chemistry, Ilam University, Ilam (Iran, Islamic Republic of); Pourmortazavi, Seied Mahdi [Faculty of Material and Manufacturing Technologies, Malek Ashtar University of Technology, Tehran (Iran, Islamic Republic of)

    2013-03-15

    Highlights: ► Synthesis of zinc oxalate nanoparticles via electrolysis of a zinc plate anode in sodium oxalate solutions. ► Design of a Taguchi orthogonal array to identify the optimal experimental conditions. ► Controlling the size and shape of particles via applied voltage and oxalate concentration. ► Characterization of zinc oxalate nanoparticles by SEM, UV–vis, FT-IR and TG–DTA. - Abstract: A rapid, clean and simple electrodeposition method was designed for the synthesis of zinc oxalate nanoparticles. Zinc oxalate nanoparticles in different size and shapes were electrodeposited by electrolysis of a zinc plate anode in sodium oxalate aqueous solutions. It was found that the size and shape of the product could be tuned by electrolysis voltage, oxalate ion concentration, and stirring rate of electrolyte solution. A Taguchi orthogonal array design was designed to identify the optimal experimental conditions. The morphological characterization of the product was carried out by scanning electron microscopy. UV–vis and FT-IR spectroscopies were also used to characterize the electrodeposited nanoparticles. The TG–DTA studies of the nanoparticles indicated that the main thermal degradation occurs in two steps over a temperature range of 350–430 °C. In contrast to the existing methods, the present study describes a process which can be easily scaled up for the production of nano-sized zinc oxalate powder.

  19. 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

  20. 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

  1. 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.

  2. Electrochemical Synthesis and Characterization of Zinc Sulfide Nanoparticles

    Directory of Open Access Journals (Sweden)

    M. Rahimi-Nasarabadi

    2014-04-01

    Full Text Available Electrosynthesis process has been used for preparation of zinc sulfide nanoparticles. Zinc sulfide nanoparticles in different size and shapes were electrodeposited by electrolysis of zinc plate as anode in sodium sulfide solution. Effects of several reaction variables, such as electrolysis voltage, sulfide ion concentration as reactant, stirring rate of electrolyte solution and temperature on particle size of prepared zinc sulfide were investigated. The significance of these parameters in tuning the size of zinc sulfide particles was quantitatively evaluated by analysis of variance (ANOVA. Also, optimum conditions for synthesis of zinc sulfide nanoparticles via electrosynthesis reaction were proposed. The structure and composition of prepared nanoparticles under optimum condition was characterized by X-ray diffraction (XRD, scanning electron microscopy (SEM, transmission electron microscopy (TEM, and UV-Vis spectrophotometry techniques.

  3. 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.

  4. 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.

  5. Continuous Preparation of Water-Dispersible Magnetite Nanoparticles by Electrochemical Synthesis.

    Science.gov (United States)

    Kim, Do-Hyeong; Park, Jin-Soo; Kang, Moon-Sung

    2018-08-01

    Highly water-dispersible magnetic nanoparticles were synthesized by convenient electrochemical techniques using a continuous flow reactor. The surface properties of the magnetic nanoparticles (MNPs) were modified with hydrophilic organic ligands during the electrochemical synthesis process to control the degree of dispersion in water. The kind of hydrophilic low-molecular weight polymers or surfactants influenced the sizes of the particles ranged between 25-40 nm (in diameter) and their size distribution. Chitosan-modified MNPs exhibited the most uniform particle size distribution among the MNPs synthesized in this study as well as excellent dispersion stability and magnetic properties in water after the crosslinking of the amino groups in chitosan. Especially, the dispersion stability of the MNPs in water was systematically investigated via a light scattering analysis.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. Thio- and Semicarbazones: Hope in the Search for Treatment of Leishmaniasis and Chagas Disease.

    Science.gov (United States)

    Silva, Barbara V; Silva, Bianca N M

    2017-01-01

    Trypanosomiasis and leishmaniasis cause severe infections in humans and domestic animals in the tropics. Although typical diseases in Latin America, globalization and the migration of infected people has spread these diseases to countries in North America, Asia and Europe. Currently available drugs are not effective in the chronic phase, as well as cause side effects and develop resistance. Among the chemical groups studied as potential anti-T. cruzi and anti-Leishmania are the thio-and semicarbazones, which are easy to obtain, possess structural versatility and can sequester metal. In this article, we present an overview of thio-and semicarbazones associated with heterocycles, indanones, and styryl and aryl skeletons, including their metal complexes with antimony, platinum, palladium, copper, ruthenium, rhenium, manganese and vanadium. Because of the efficiency and selectivity that some of these derivatives have shown, it can be concluded that thio-and semicarbazones constitute promising chemical scaffolds in the search for new anti-parasitic agents. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  11. Synthesis, characterization and electrochemical study of Mn-doped TiO2 decorated polypyrrole nanotubes

    Science.gov (United States)

    Saidur, M. R.; Aziz, A. R. Abdul; Basirun, W. J.

    2017-06-01

    Nanostructured conductive polymers are the growing interest in the field of electrochemistry due to their superior conductivity and environmental friendliness. The existence of transition metal oxides could improve their nanostructure as well as conductive properties. In this study, polypyrrole nanotubes are synthesized in the presence of TiO2 and manganese (Mn)-doped TiO2 nanoparticles (NPs) to investigate their electrochemical properties. Details characterization of the synthesized composites were done by X-Ray diffraction (XRD) and TEM. The TEM analysis shows that doping of TiO2 with Mn decrease the grain size of the TiO2 nanoparticles and successively its effects on the synthesis of the PPy nanotubes (PPyNTs). TEM confirmed that PPyNTs synthesized in the presence of Mn-doped TiO2 are thinner in size compare to the PPyNTs synthesized in presence of pure TiO2. The electrochemical effectiveness of the synthesized PPy nanocomposite was investigated using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). CV and EIS both on a modified glassy carbon electrode reveal the better electron transportability for the Mn-doped TiO2 PPyNTs due to the synergistic effect of doping and decreased the size of PPyNTs as well as increased surface area.

  12. Influence of the temperature in the electrochemical synthesis of cobalt ferrites nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Mazario, E. [Departamento de Quimica Fisica Aplicada, Facultad de Ciencias, Universidad Autonoma de Madrid, UAM, C/Francisco Tomas y Valiente 7, 28049 Cantoblanco, Madrid (Spain); Morales, M.P. [Instituto de Ciencia de Materiales de Madrid, CSIC, C/Sor Juana Ines de la Cruz 3, 28049 Cantoblanco, Madrid (Spain); Galindo, R. [Departamento de Quimica Fisica Aplicada, Facultad de Ciencias, Universidad Autonoma de Madrid, UAM, C/Francisco Tomas y Valiente 7, 28049 Cantoblanco, Madrid (Spain); Herrasti, P., E-mail: pilar.herrasti@uam.es [Departamento de Quimica Fisica Aplicada, Facultad de Ciencias, Universidad Autonoma de Madrid, UAM, C/Francisco Tomas y Valiente 7, 28049 Cantoblanco, Madrid (Spain); Menendez, N. [Departamento de Quimica Fisica Aplicada, Facultad de Ciencias, Universidad Autonoma de Madrid, UAM, C/Francisco Tomas y Valiente 7, 28049 Cantoblanco, Madrid (Spain)

    2012-09-25

    Highlights: Black-Right-Pointing-Pointer Cobalt ferrite nanoparticles were synthesized by new electrochemical method. Black-Right-Pointing-Pointer Temperature affects to percentage of inclusion of Co and diameter of the synthesized nanoparticles. Black-Right-Pointing-Pointer At 80 Degree-Sign C and current densities of 50/25 mA cm{sup -2} applied to Fe and Co, respectively, a stoichiometric CoFe{sub 2}O{sub 4} nanoparticles with 40 nm of diameter were obtained. - Abstract: A new electrochemical method to synthesize cobalt ferrite nanoparticles has been developed. Magnetic measurement, Moessbauer spectroscopy, X-ray diffraction, inductive coupled plasma spectroscopy, and transmission electron microscopy were carried out to characterize the cobalt ferrites synthesized at different temperatures between 25 Degree-Sign C and 80 Degree-Sign C. These techniques confirm the efficiency of the electrochemical method. At room temperature a mixture of different compounds was obtained with a particle diameter around 20 nm, while at 80 Degree-Sign C the synthesis of cobalt ferrite leads to a stoichiometric spinel, with a crystallite size of 40 nm measured by Scherrer equation. The temperature was defined as an important parameter to obtain stoichiometric ferrites and different diameters.

  13. 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.

  14. 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.

  15. 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...... galvanic industries....

  16. Polymers containing nickel(II) complexes of Goedken's macrocycle: optimized synthesis and electrochemical characterization.

    Science.gov (United States)

    Paquette, Joseph A; Sauvé, Ethan R; Gilroy, Joe B

    2015-04-01

    The synthesis and characterization of a new class of nickel-containing polymers is described. The optimized copolymerization of alkyne-bearing nickel(II) complexes of Goedken's macrocycle (4,11-dihydro-5,7,12,14-tetramethyldibenzo[b,i][1,4,8,11]tetraazacyclotetradecine) and brominated 9,9-dihexylfluorene produced polymers with potential application as functional redox-active materials. The title polymers exhibit electrochemically reversible, ligand-centered oxidation events at 0.24 and 0.73 V versus the ferrocene/ferrocenium redox couple. They also display exceptional thermal stability and interesting absorption properties due to the presence of the macrocyclic nickel(II) complexes and π-conjugated units incorporated in their backbones. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. 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.

  18. Electrochemical activation of carbon dioxide for synthesis of dimethyl carbonate in an ionic liquid

    International Nuclear Information System (INIS)

    Yuan Dandan; Yan Cuihong; Lu Bin; Wang Hongxia; Zhong Chongmin; Cai Qinghai

    2009-01-01

    The direct synthesis of dimethyl carbonate from methanol and carbon dioxide is challenging due to the thermodynamic stability and kinetic inertness of CO 2 . Electrochemical technique can overcome this challenge by providing a method for preliminary activation of CO 2 . Electrocatalytic activation and conversion of carbon dioxide to dimethyl carbonate with platinum electrodes in a dialkylimidazolium ionic liquids-basic compounds-methanol system was conducted under ambient conditions. Among the basic compounds and ionic liquids, CH 3 OK acts as a co-catalyst and 1-butyl-3-methylimidazolium bromide (bmimBr) acts as an electrolyte. In the bmimBr-CH 3 OK-methanol system, the absence of CH 3 I and/or any other organic additives allows dimethyl carbonate to be effectively synthesized. The reaction mechanism proposed here is different from those previously reported

  19. 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.

  20. Green synthesis of 1,4-quinone derivatives and evaluation of their fluorescent and electrochemical properties

    Directory of Open Access Journals (Sweden)

    Palanisamy Ravichandiran

    2016-09-01

    Full Text Available Green synthesis of some 1,4-quinone derivatives by conventional and solvent free microwave assisted methods has been reported. The microwave assisted method resulted in higher percentage yield at shorter time compared to the conventional one. In the conventional method environmentally friendly solvent was used and the results were compared with other solvents. When water was used as a solvent the reaction exhibited higher yield than other solvents like ethanol. The solvent free method under microwave irradiation method yielded the highest yield compared to the conventional methods. The resultant compounds were analyzed by UV–Vis, FT-IR, 1H and 13C NMR spectroscopy. The synthesized quinone derivatives exhibited the fluorescent and electrochemical properties.

  1. 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.

  2. 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

  3. Synthesis and photophysical and electrochemical properties of novel unsymmetrical phthalocyanines with a Sudan IV moiety

    Science.gov (United States)

    Özçeşmeci, Ibrahim; Büyük, Pınar; Nar, Ilgın; Gül, Ahmet

    The synthesis of novel, A3B type unsymmetrical metal-free and metallophthalocyanines bearing one aza dye group Sudan IV and three nitro terminal moieties was achieved by cyclotetramerization of novel 4-((1-((E)-(2-methyl-4-((E)-o-tolyldiazenyl)phenyl)diazenyl)naphthalen-2-yl)oxy)phthalonitrile and 4-nitrophthalonitrile. The new unsymmetrical metal-free and metallophthalocyanines have been characterized using elemental analyses, 1H NMR, FT-IR, UV-vis and mass spectroscopic data. The aggregation properties of the compounds were investigated in a concentration range of 1.0 × 10‑4 M-6.25 × 10‑6 M. General trends were also studied for fluorescence quantum yields and lifetimes of these phthalocyanine compounds in tetrahydrofuran. The fluorescence of the synthesized unsymmetrical metal-free and metallophthalocyanines is effectively quenched by 1,4-benzoquinone (BQ) in THF. In-depth investigation of the electrochemical properties showed that nitro groups extended the reduction potentials. The synthesis of novel, A3B type unsymmetrical metal-free and metallo phthalocyanines bearing one aza dye group Sudan IV and three nitro terminal moieties was achieved by cyclotetramerization of novel 4-((1-((E)-(2-methyl-4-((E)-o-tolyldiazenyl)phenyl)diazenyl) naphthalen-2-yl)oxy)phthalonitrile and 4-nitrophthalonitrile. The aggregation properties of the compounds were investigated. General trends were also studied for fluorescence quantum yields and lifetimes of these phthalocyanine compounds. In-depth investigation of the electrochemical properties showed that nitro groups extended the reduction potentials.

  4. Silver/poly(N-vinyl-2-pyrrolidone nanocomposites obtained by the electrochemical synthesis

    Directory of Open Access Journals (Sweden)

    Jovanović Željka

    2011-01-01

    Full Text Available Silver/poly(N-vinyl-2-pyrrolidone (Ag/PVP nanocomposites were obtained by electrochemical reduction of Ag+ ions at a constant voltage, by the in situ synthesis of silver nanoparticles inside poly(N-vinyl-2-pyrrolidone matrix, previously crosslinked by γ-irradiation. Optimal values of synthesis parameters were investigated: the composition of the solution for swelling of PVP hydrogel, implementation time and applied voltage. Ag/PVP nanocomposites were characterized by UV-visible spectroscopy, and IR spectroscopy. UV-visible spectroscopy results shown that the reduction of silver ions was more efficient when the more conductive solution for swelling of PVP hydrogel was used, i.e. the solution containing 3.9 mM AgNO3 with 0.1 M KNO3. Also, it was shown that the concentration of the reduced silver increases with the increase in implementation time and applied voltage, up to the values of 4 min, and 200 V, respectively. The Ag nanoparticle size was estimated to be 25 nm, by comparison of the experimental results of UV-vis spectroscopy with the theoretical predictions obtained by the calculations in “MiePlot v.3.4” computer program, having the algorithm based on Mie scattering from a sphere. The results of FTIR spectroscopy have shown that Ag nanoparticles are mainly bonded to PVP by coordination bondages between Ag nanoparticles and N from the pyrrolidone ring of PVP.

  5. 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%.

  6. 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.

  7. 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

  8. Electrochemical synthesis of Poly[3, 4-Propylenedioxythiophene-co-N-Phenylsulfonyl Pyrrole]: Morphological, electrochemical and spectroscopic characterization

    Directory of Open Access Journals (Sweden)

    2011-06-01

    Full Text Available Electroactive random copolymers of 3,4-Propylenedioxythiophene (ProDOT and N-Phenylsulfonyl Pyrrole (PSP were electrochemically synthesized on single carbon fiber microelectrode (SCFME by cyclic voltammetry (CV. Fourier Transform Infrared-Attenuated Total Reflectance (FTIR-ATR measurements indicate the inclusion of PSP into the copolymer structure. The influence of feed ratios on the copolymers was studied by CV and electrochemical impedance spectroscopy (EIS and equivalent circuit modelling (ECM. The morphologies and film thicknesses of copolymers were characterized by scanning electron microscopy (SEM and atomic force microscopy (AFM. The results have shown that the principal changes in morphology, conductivity, porous nature and thickness of Poly(ProDOT-co-PSP film depend on the concentration of PSP. The strong electron-withdrawing sulfonyl group substitution on PSP significantly inhibited electrochemical copolymerization. Semicircular characteristics at Nyquist plots reflected an increasing trend with the increase of PSP concentration in the feed at high frequency. The semicircular characteristic of the copolymer film is useful for the bioelectrochemical sensor applications.

  9. Silver Nanoparticles Mediated by Costus afer Leaf Extract: Synthesis, Antibacterial, Antioxidant and Electrochemical Properties.

    Science.gov (United States)

    Elemike, Elias E; Fayemi, Omolola E; Ekennia, Anthony C; Onwudiwe, Damian C; Ebenso, Eno E

    2017-04-29

    Synthesis of metallic and semiconductor nanoparticles through physical and chemical routes has been extensively reported. However, green synthesized metal nanoparticles are currently in the limelight due to the simplicity, cost-effectiveness and eco-friendliness of their synthesis. This study explored the use of aqueous leaf extract of Costus afer in the synthesis of silver nanoparticles (CA-AgNPs). The optical and structural properties of the resulting silver nanoparticles were studied using UV-visible spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Fourier transform infra-red spectrophotometer (FTIR). TEM images of the silver nanoparticles confirmed the existence of monodispersed spherical nanoparticles with a mean size of 20 nm. The FTIR spectra affirmed the presence of phytochemicals from the Costus afer leaf extract on the surface of the silver nanoparticles. The electrochemical characterization of a CA-AgNPs/multiwalled carbon nanotubes (MWCNT)-modified electrode was carried out to confirm the charge transfer properties of the nanocomposites. The comparative study showed that the CA-AgNPs/MWCNT-modified electrode demonstrated faster charge transport behaviour. The anodic current density of the electrodes in Fe(CN)₆] 4- /[Fe(CN)₆] 3- redox probe follows the order: GCE/CA-Ag/MWCNT (550 mA/cm²) > GCE/MWCNT (270 mA/cm²) > GCE (80 mA/cm²) > GCE/CA-Ag (7.93 mA/cm²). The silver nanoparticles were evaluated for their antibacterial properties against Gram negative ( Escherichia coli, Klebsiella pneumonia, Pseudomonas aeruginosa ) and Gram positive ( Bacillus subtilis and Staphylococcus aureus ) pathogens. The nanoparticles exhibited better inhibition of the bacterial strains compared to the precursors (leaf extract of Costus afer and silver nitrate). Furthermore, the ability of the nanoparticles to scavenge DPPH radicals at different concentrations was studied using the DPPH radical scavenging assay and compared to

  10. Silver Nanoparticles Mediated by Costus afer Leaf Extract: Synthesis, Antibacterial, Antioxidant and Electrochemical Properties

    Directory of Open Access Journals (Sweden)

    Elias E. Elemike

    2017-04-01

    Full Text Available Synthesis of metallic and semiconductor nanoparticles through physical and chemical routes has been extensively reported. However, green synthesized metal nanoparticles are currently in the limelight due to the simplicity, cost-effectiveness and eco-friendliness of their synthesis. This study explored the use of aqueous leaf extract of Costus afer in the synthesis of silver nanoparticles (CA-AgNPs. The optical and structural properties of the resulting silver nanoparticles were studied using UV-visible spectroscopy, scanning electron microscopy (SEM, transmission electron microscopy (TEM and Fourier transform infra–red spectrophotometer (FTIR. TEM images of the silver nanoparticles confirmed the existence of monodispersed spherical nanoparticles with a mean size of 20 nm. The FTIR spectra affirmed the presence of phytochemicals from the Costus afer leaf extract on the surface of the silver nanoparticles. The electrochemical characterization of a CA-AgNPs/multiwalled carbon nanotubes (MWCNT-modified electrode was carried out to confirm the charge transfer properties of the nanocomposites. The comparative study showed that the CA-AgNPs/MWCNT-modified electrode demonstrated faster charge transport behaviour. The anodic current density of the electrodes in Fe(CN6]4−/[Fe(CN6]3− redox probe follows the order: GCE/CA-Ag/MWCNT (550 mA/cm2 > GCE/MWCNT (270 mA/cm2 > GCE (80 mA/cm2 > GCE/CA-Ag (7.93 mA/cm2. The silver nanoparticles were evaluated for their antibacterial properties against Gram negative (Escherichia coli, Klebsiella pneumonia, Pseudomonas aeruginosa and Gram positive (Bacillus subtilis and Staphylococcus aureus pathogens. The nanoparticles exhibited better inhibition of the bacterial strains compared to the precursors (leaf extract of Costus afer and silver nitrate. Furthermore, the ability of the nanoparticles to scavenge DPPH radicals at different concentrations was studied using the DPPH radical scavenging assay and compared to

  11. 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.

  12. 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

  13. 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.

  14. Synthesis and Electrochemical Characterization of Ni Nanoparticles by Hydrazine Reduction using Hydroxyethyl cellulose as Capping Agent

    International Nuclear Information System (INIS)

    Ramírez-Meneses, E.; Torres-Huerta, A.M.; Domínguez-Crespo, M.A.; Ponce-Varela, M.G.; Hernández-Pérez, M.A.; Betancourt, I.; Palacios-González, E.

    2014-01-01

    The controlled-size synthesis of well-dispersed metal nanoparticles has been the aim of many research works during the last two decades. In this context, simple and controlled methods are the most suitable to obtain metal nanoparticles. The reduction of transition metal salts in solution is the most widely used method for generating colloidal suspensions of metals. In this work, nickel nanoparticles were synthesized from NiCl 2 ·6H 2 O in an ethanol solution with hydrazine hydrate and an appropriate amount of NaOH in the presence of hydroxyethyl cellulose (HEC) used as a capping agent to avoid the coalescence of the nanostructures. Size effects on the nickel nanostructures were studied by varying the concentration of the reducing agent and temperature. The obtained nickel nanostructures were characterized by X-ray diffraction (XRD), showing a face-centered cubic (fcc) structure. Particle sizes from 7 to 13 nm were determined by the Scherrer equation. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) showed spherical sponge-like nanostructures formed by thin laminar structures. Additionally, infrared spectroscopy showed the presence of HEC functional groups on the surface of the nickel nanostructures after the purification step. Finally, the obtained Ni nanostructures were also characterized by electrochemical techniques and magnetic measurements to determine their electrocatalytic properties and magnetic response, respectively

  15. 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.

  16. Phenylalanine-Rich Peptide Mediated Binding with Graphene Oxide and Bioinspired Synthesis of Silver Nanoparticles for Electrochemical Sensing

    Directory of Open Access Journals (Sweden)

    Li Wang

    2017-02-01

    Full Text Available We demonstrated that a phenylalanine-rich peptide molecule, (FEFEFKFK2, could be used for the biofunctionalization of graphene oxide (GO and the bioinspired synthesis of silver nanoparticles (AgNPs for the creation of functional GO–AgNPs nanohybrids. The successful synthesis of GO–AgNPs nanohybrids was proven by the characterizations of atomic force microscopy, transmission electron microscope, and X-ray photoelectron spectroscopy. The fabricated electrochemical H2O2 sensor based on the synthesized GO–AgNPs nanohybrids showed high performances with a linear detection range 0.02–18 mM and a detection limit of 0.13 μM. The design of graphene-binding peptides is of benefit to the biofunctionalization of graphene-based materials, the synthesis of novel graphene–peptide nanohybrids, and the potential applications of graphene in biomedical fields.

  17. Study of the aqueous synthesis, optical and electrochemical characterization of alloyed ZnxCd1-xTe nanocrystals

    International Nuclear Information System (INIS)

    Matos, Charlene Regina Santos; Candido, Luan P.M.; Souza, Helio Oliveira; Pereira da Costa, Luiz; Sussuchi, Eliana Midori; Gimenez, Iara F.

    2016-01-01

    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 x Cd 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.

  18. Hierarchically structured carbon-based composites: Design, synthesis and their application in electrochemical capacitors.

    Science.gov (United States)

    Yuan, C Z; Gao, B; Shen, L F; Yang, S D; Hao, L; Lu, X J; Zhang, F; Zhang, L J; Zhang, X G

    2011-02-01

    This feature article provides an overview of the recent research progress on the hierarchically structured carbon-based composites for electrochemical capacitors. The basic principles of electrochemical capacitors, and the design, construction and performance of hierarchically structured carbon-based composites electrode materials with good ions and electron transportation and large specific surface area are discussed. The trend of future development of high-power and large-energy electrochemical capacitors is proposed.

  19. Thiosemicarbazones, semicarbazones, dithiocarbazates and hydrazide/hydrazones: anti-Mycobacterium tuberculosis activity and cytotoxicity.

    Science.gov (United States)

    Pavan, Fernando R; da S Maia, Pedro I; Leite, Sergio R A; Deflon, Victor M; Batista, Alzir A; Sato, Daisy N; Franzblau, Scott G; Leite, Clarice Q F

    2010-05-01

    The aim of this study was to identify a candidate drug for the development of anti-tuberculosis therapy from previously synthesized compounds based on the thiosemicarbazones, semicarbazones, dithiocarbazates and hydrazide/hydrazones compounds. The minimal inhibitory concentration (MIC) of these compounds against Mycobacterium tuberculosis was determined. Their in vitro cytotoxicity to J774 cells (IC50) was determined to establish a selectivity index (SI) (SI=IC50/MIC). The best compounds were the thiosemicarbazones (2, 3 and 4) and the hydrazide/hydrazones (14, 15, 16 and 18). The results are comparable to or better than those of "first line" or "second line" drugs commonly used to treat TB, suggesting these compounds as anti-TB drug candidates. Copyright (c) 2010 Elsevier Masson SAS. All rights reserved.

  20. FT-IR, FT-Raman and Computational Study of Ethyl Methyl Ketone Semicarbazone

    Directory of Open Access Journals (Sweden)

    P. S. Binil

    2011-01-01

    Full Text Available FT-IR and FT-Raman spectra of ethyl methyl ketone semicarbazone were recorded and analyzed. The vibrational wavenumbers were computed using HF/6-31G*, B3PW91/6-31G* and B3LYP/6-31G* basis and compared with experimental data. The first hyperpolarizability, infrared intensities and Raman activities are reported. The calculated first hyperpolarizability is comparable with the reported values of similar derivatives and is an attractive object for future studies of non-linear optics. The extended π-electron delocalization over the carbazone moiety is responsible for the nonlinearity of the molecule. The geometrical parameters of the title compound are in agreement with that of similar derivatives. The red shift of the NH stretching wavenumber in the infrared spectrum from the computed wavenumber indicates the weakening of the NH bond resulting in proton transfer to the neighboring oxygen atom.

  1. Electrochemical synthesis and characterization of BaB6 from molten melt

    Directory of Open Access Journals (Sweden)

    Jose T.P.

    2009-01-01

    Full Text Available Barium hexaboride (BaB6 crystals were electrochemically synthesized using molten salt technique. Barium carbonate (BaCO3 and boron trioxide (B2O3 was used as reactants. Lithium fluoride (LiF was used as the supporting electrolyte. The molten electrolyte consisted of 50 wt % BaCO3 and B2O3 with different stiochiometric ratios of Ba and B and 50 wt % lithium fluoride. DTA/TGA studies were made to determine the eutectic point of the melt and it was found to be around 821oC. The electrolytic cell had a high purity graphite crucible, which served as the electrolyte holding vessel and also as the anode for the electrolysis. An electro-polished molybdenum rod was employed as the cathode. The electrolysis was performed at 870ºC under argon atmosphere, at current densities ranging from 0.2-0.5 A/cm2. The electrodeposited crystals were examined for the phase identification using X-ray diffraction technique. The AAS and the chemical analysis were made for the determination of chemical composition of the synthesized crystals. The purity of the crystals was also assessed using ICP-MS, XRF and EDX, which reveal that the crystals were associated with trace amount of impurities like oxygen, carbon and iron. The compound is found to be more than 99 % pure. The morphology of the crystals was examined using Scanning Electron Microscopy (SEM. From the above studies, it is concluded that the molten salt process is a simple preparative procedure for the synthesis of sub-micron size barium hexaboride crystals.

  2. Electrochemical Synthesis of Binary and Ternary Niobium-Containing Oxide Electrodes Using the p-Benzoquinone/Hydroquinone Redox Couple.

    Science.gov (United States)

    Papa, Christopher M; Cesnik, Anthony J; Evans, Taylor C; Choi, Kyoung-Shin

    2015-09-01

    New electrochemical synthesis methods have been developed to obtain layered potassium niobates, KNb3O8 and K4Nb6O17, and perovskite-type KNbO3 as film-type electrodes. The electrodes were synthesized from aqueous solutions using the redox chemistry of p-benzoquinone and hydroquinone to change the local pH at the working electrode to trigger deposition of desired phases. In particular, the utilization of electrochemically generated acid via the oxidation of hydroquinone for inorganic film deposition was first demonstrated in this study. The layered potassium niobates could be converted to (H3O)Nb3O8 and (H3O)4Nb6O17 by cationic exchange, which, in turn, could be converted to Nb2O5 by heat treatment. The versatility of the new deposition method was further demonstrated for the formation of CuNb2O6 and AgNbO3, which were prepared by the deposition of KNb3O8 and transition metal oxides, followed by thermal and chemical treatments. Considering the lack of solution-based synthesis methods for Nb-based oxide films, the methods reported in this study will contribute greatly to studies involving the synthesis and applications of Nb-based oxide electrodes.

  3. 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)

  4. Electrochemical synthesis and characterisation of hybrid materials polypyrrole/dodecatungstophosphate as protective agents against steel corrosion

    Science.gov (United States)

    Bonastre Cano, Jose Antonio

    hand, this pretreatment should guarantee appropriate conditions in order to obtain a coating with high adhesion on carbon steel. Once studied the better parameters for the synthesis of the hybrid material by cyclic voltammetry, hybrid material is morphological, chemical and electrochemical characterised by the following techniques: Cyclic Voltammetry, Scanning Electron Microscopy, Energy Dispersive X Ray, X Ray Photoelectron Spectroscopy and Electrochemical Impedance Spectroscopy. The hybrid material polypyrrole/PW 12O403-. chemical structure presents Fe oxides and hydroxide within the polypyrrole polycationic matrix. Hybrid material polypyrrol/PW12O403- diminishes the corrosion of carbon steel in NaOH and Porland cement filtering solutions. These cement solutions simulate the pore fluid conditions existing in cured mortar or concrete elements. Fe ion concentration data were determinated in corrosion tests. Voltammetric response of polymeric coatings was evaluated by cyclic voltammetry. Finally, the protection provided by hybrid material polypyrrole/PW 12O403, in oxidised and reduced state, was evaluated on carbon steel electrodes embedded in Portland cement mortars immersed in seawater and submitted to an accelerated carbonation process for 265 days. Polymeric material covered carbon steel electrodes in reduced state suffer a Fe gravimetric loss 15 times lower than the ones of bare electrodes against chlorides attack, due to the effect of physical barrier. Hybrid material covered electrodes in oxidised state after being submitted to a carbonation process suffer a Fe gravimetric loss 2.5 times lower than the ones of bare electrodes, due to galvanic protection provided by hybrid material polypyrrole/PW 12O403- on carbon steel.

  5. Synthesis and characterization of CoFe2O4 ferrite nanoparticles obtained by an electrochemical method.

    Science.gov (United States)

    Mazarío, E; Herrasti, P; Morales, M P; Menéndez, N

    2012-09-07

    Uniform size cobalt ferrite nanoparticles have been synthesized in one step using an electrochemical technique. Synthesis parameters such as the current density, temperature and stirring were optimized to produce pure cobalt ferrite. The nanoparticles have been investigated by means of magnetic measurements, Mössbauer spectroscopy, x-ray powder diffraction and transmission electron microscopy. The average size of the electrosynthesized samples was controlled by the synthesis parameters and this showed a rather narrow size distribution. The x-ray analysis shows that the CoFe(2)O(4) obtained presents a totally inverse spinel structure. The magnetic properties of the stoichiometric nanoparticles show ferromagnetic behavior at room temperature with a coercivity up to 6386 Oe and a saturation magnetization of 85 emu g(-1).

  6. 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.

  7. 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.

  8. 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.

  9. 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

  10. Electrochemical synthesis of mesoporous CoPt nanowires for methanol oxidation

    OpenAIRE

    Serrà, Albert; Montiel Argaiz, Manuel; Gómez, Elvira; Vallés Giménez, Elisa

    2014-01-01

    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)...

  11. Direct Electrochemical Synthesis of Bismuth(III Phenoxides and their Coordination Compounds

    Directory of Open Access Journals (Sweden)

    Harpreet Kaur

    2012-01-01

    Full Text Available Bismuth(III phenoxides have been synthesized by electrochemical reactions of 1-naphthol, 2-naphthol, 4-aminophenol, 2-nitrophenol, 4-nitrophenol, 2-hydroxybenzoic acid, p-cresol, phenol, resorcinol, 2-tert-butylphenol and 2-tert-butyl-4-methoxyphenol at sacrificial bismuth anode and inert platinum cathode using tetrabutylammonium chloride as supporting electrolyte. The coordination compounds of these phenols with 1, 10-phenanthroline and 2, 2ʼ-bipyridyl have also been synthesized electrochemically. The solid products separated in the anode compartment have been isolated and characterized by elemental analysis and infrared spectral studies. Current efficiencies of these reactions are quite high.

  12. 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

  13. Mg(II Selective PVC Membrane Electrode Based on Methyl Phenyl Semicarbazone as an Ionophore

    Directory of Open Access Journals (Sweden)

    Sulekh Chandra

    2013-01-01

    Full Text Available A PVC-membrane-based Mg(II selective electrode was constructed using methyl phenyl semicarbazone (MPS as a neutral carrier. The sensor exhibits a Nernstian response for Mg(II ion over a wide concentration range 1.0×10-8  to  1.0×10-1 M with the slope of 28.4 mV/per decade having detection limit 1.7×10-9 M. It was relatively a fast response time (<10 s for concentration ≥1.0×10-3 and <15 s for concentration of ≥1.0×10-6 M and can be used for 8 months without any considerable divergence in potentials. The proposed sensor revealed relatively good selectivity and high sensitivity for Mg(II over a mono-, di-, and trivalent cation and can be used in a pH range of 1.0–9.5. It was also successfully used as an indicator electrode in potentiometer titration and in the analysis of concentration of magnesium in various real samples.

  14. Fulleropyrrolidine end-capped molecular wires for molecular electronics--synthesis, spectroscopic, electrochemical, and theoretical characterization

    DEFF Research Database (Denmark)

    Sørensen, Jakob Kryger; Fock, Jeppe; Pedersen, Anders Holmen

    2011-01-01

    -withdrawing ester group present. The effect of extending the p-system of the central wire from 1,4-phenylenediamine to 2,7-fluorenediamine was investigated by absorption, fluorescence, and electrochemical methods. The central wire and the C(60) end-groups were found not to electronically communicate in the ground...

  15. 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.

  16. 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

  17. 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.

  18. Electrochemical synthesis of Mo{sub 2}C catalytical coatings for the water-gas shift reaction

    Energy Technology Data Exchange (ETDEWEB)

    Kuznetsov, S.A.; Dubrovskiy, A.R. [Inst. of Chemistry, Kola Science Centre RAS, Apatity, Murmansk Region (Russian Federation); Rebrov, E.V.; Schouten, J.C. [Lab. of Chemical Reactor Engineering, Eindhoven Univ. of Tech., Eindhoven (Netherlands)

    2007-10-15

    The electroreduction of CO{sub 3}{sup 2-} ions on a molybdenum cathode in a NaCl-KCl-Li{sub 2}CO{sub 3} melt was studied by cyclic voltammetry. The electrochemical synthesis of Mo{sub 2}C on molybdenum substrates has been performed at 1123 K for 7 h with a cathodic current density of 5 mA cm{sup -2}. If molybdenum carbide is present as a thin (ca. 500 nm) film on a molybdenum substrate (Mo{sub 2}C/Mo), its catalytic activity in the water gas-shift reaction is enhanced by at least an order of magnitude compared to that of the bulk Mo{sub 2}C phase. (orig.)

  19. 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)

  20. 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)

  1. In Situ Electrochemical Synthesis of Oriented and Defect-Free AEL Molecular-Sieve Films Using Ionic Liquids.

    Science.gov (United States)

    Yu, Tongwen; Chu, Wenling; Cai, Rui; Liu, Yanchun; Yang, Weishen

    2015-10-26

    Simply preparing oriented and defect-free molecular-sieve films have been a long-standing challenge both in academia and industry. Most of the early works focus on the careful and multiple controls of the seeds layer or synthesis conditions. Herein, we report a one-step in situ electrochemical ionothermal method that combines a controllable electric field with ionic liquids. We demonstrate that an in-plane oriented and defect-free AEL (one molecular-sieve framework type) molecular-sieve film was obtained using an Al electrode as the Al source. The excellent corrosion-resistant performance of the film makes this technology promising in multiple applications, such as anti-corrosion coatings. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. 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.

  3. 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.

  4. Facile synthesis of reduced graphene oxide-modified, nitrogen-doped carbon xerogel with enhanced electrochemical capacitance

    Energy Technology Data Exchange (ETDEWEB)

    Lei, Gang [College of Chemistry and Chemical Engineering, Central South University, Changsha 410083 (China); Hu, Xiaoyong [College of Chemistry and Chemical Engineering, Hunan University, Changsha 410082 (China); Peng, Zhiguang [College of Chemistry and Chemical Engineering, Central South University, Changsha 410083 (China); Hu, Jiawen, E-mail: jwhu@hnu.edu.cn [College of Chemistry and Chemical Engineering, Hunan University, Changsha 410082 (China); Liu, Hongtao, E-mail: liuht@csu.edu.cn [College of Chemistry and Chemical Engineering, Central South University, Changsha 410083 (China)

    2014-12-15

    In this contribution, we report a reduced graphene oxide (rGO)-modified nitrogen-doped carbon xerogel, which could be easily prepared by pyrolysis of melamine-formaldehyde (MF) resins that are polymerized hydrothermally in an aqueous GO dispersion. Scanning electron microscopy, transmission electron microscopy, Fourier-transformed infrared spectrometry, and nitrogen adsorption-desorption method were employed to reveal the morphologies and structures of the prepared carbon xerogel. Cyclic voltammetry, electrochemical impedance spectroscopy, and galvanostatic charge–discharge were used to investigate the electrochemical properties. The results showed that the charge transfer barrier of the mesoporous nitrogen-doped carbon xerogel was decreased evidently, owing to the modification of a layer of rGO on its wall, and the xerogel demonstrated a capacitance of as high as 205 F g{sup −1} at the current of 1 A g{sup −1}. - Graphical abstract: A facile synthesis of rGO-modified, N-doped carbon material for supercapacitor application. - Highlights: • Nitrogen-doping and graphene-attachment in the carbon material are simultaneously achieved. • A thin layer of graphene attached on the wall of the mesoporous carbon material speeds up the charge transfer. • The graphene-modified nitrogen-doped carbon xerogel shows great potential for supercapacitor application.

  5. Electrochemical synthesis of NiFe{sub 2}O{sub 4} nanoparticles: Characterization and their catalytic applications

    Energy Technology Data Exchange (ETDEWEB)

    Galindo, R. [Chemistry Department, Universidad de Guanajuato, Cerro de la Venada S/N, Pueblito de Rocha, C.P. 36040 Guanajuato Gto. (Mexico); Department of Physical Chemistry Applied, Universidad Autonoma de Madrid, Cantoblanco S/N, C.P 28049 Madrid (Spain); Mazario, E. [Department of Physical Chemistry Applied, Universidad Autonoma de Madrid, Cantoblanco S/N, C.P 28049 Madrid (Spain); Gutierrez, S. [Chemistry Department, Universidad de Guanajuato, Cerro de la Venada S/N, Pueblito de Rocha, C.P. 36040 Guanajuato Gto. (Mexico); Morales, M.P. [Materials Science Institute of Madrid, Sor Juana Ines de la Cruz 3, Cantoblanco, 28049 Madrid (Spain); Herrasti, P., E-mail: pilar.herrasti@uam.es [Department of Physical Chemistry Applied, Universidad Autonoma de Madrid, Cantoblanco S/N, C.P 28049 Madrid (Spain)

    2012-09-25

    Highlights: Black-Right-Pointing-Pointer Nickel ferrite nanoparticles were synthesized by new electrochemical method. Black-Right-Pointing-Pointer Stoichometric nanoparticles with 20 nm of size can be prepared with this method. Black-Right-Pointing-Pointer Nickel ferrites nanoparticles were used as catalysts in the direct oxidation of glucose at pH 7. - Abstract: In this work a new route for preparation of nickel ferrites nanoparticles has been developed. The synthesis is carried out in an electrochemical cell using three electrodes, a sheet of iron was employed as cathode and two sheets of iron and nickel were used as sacrificial anodes. The obtained nanoparticles were washed several times with distilled water, separated magnetically and dried under vacuum with constant temperature for 12 h. The characterization of the nanoparticles was carried out by X-ray diffraction (XRD), transmission electron microscopy (TEM), and Inductively coupled plasma mass spectrometry (ICP-MS). Magnetic measurements were carried out using a vibrating sample magnetometer (VSM). To evaluate the catalytical properties of these nanoparticles against the oxidation of glucose a graphite paste electrode (GPE) was made. The proportions of the nanoparticles in GPE were 5, 10, 20 and 50% in weight. The electrode shows promising properties for its use as catalyst in the glucose oxidation.

  6. Synthesis and electrochemical oxidation of hybrid compounds: dihydropyridine-fused coumarins

    International Nuclear Information System (INIS)

    Pardo-Jiménez, V.; Barrientos, C.; Pérez-Cruz, K.; Navarrete-Encina, P.A.; Olea-Azar, C.; Nuñez-Vergara, Luis J.; Squella, J.A.

    2014-01-01

    In this paper, a series of six dihydropyridine-fused coumarins were synthesized and electrochemically characterized in dimethylformamide (DMF). Dihydropyridine ring oxidation on glassy carbon electrode (GCE) for condensed heterocyclic compounds revealed a single anodic peak. Oxidation potential values correlated fairly well with substituent effects at 9-position. The overall oxidation mechanism involved 2-electrons and 2-protons as determined by chronoamperometry. Controlled-potential electrolysis followed by UV-Visible spectroscopy proves that dihydropyridine-fused coumarins are electrochemically oxidized in DMF giving rise to the aromatic pyridine derivative. ESR experimental spectra show a triplet, due to the C-centered dihydropyridyl radical trapped with N-tert-butylamine-α-phenylnitrone (PBN). Hyperfine coupling constant values (aN) of dihydropyridine-fused coumarins were higher than corresponding values for non-fused ones. These results could be due to the effect of the coupling of the dihydropyridine moiety with the coumarin ring over the splitting constant

  7. 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.

  8. Rational synthesis of silver vanadium oxides/polyaniline triaxial nanowires with enhanced electrochemical property.

    Science.gov (United States)

    Mai, Liqiang; Xu, Xu; Han, Chunhua; Luo, Yanzhu; Xu, Lin; Wu, Yimin A; Zhao, Yunlong

    2011-11-09

    We designed and successfully synthesized the silver vanadium oxides/polyaniline (SVO/PANI) triaxial nanowires by combining in situ chemical oxidative polymerization and interfacial redox reaction based on β-AgVO(3) nanowires. The β-AgVO(3) core and two distinct layers can be clearly observed in single triaxial nanowire. Fourier transformed infrared spectroscopic and energy dispersive X-ray spectroscopic investigations indicate that the outermost layer is PANI and the middle layer is Ag(x)VO((2.5+0.5x)) (x < 1), which may result from the redox reaction of Ag(+) and aniline monomers at the interface. The presence of the Ag particle in a transmission electron microscopy image confirms the occurrence of the redox reaction. The triaxial nanowires exhibit enhanced electrochemical performance. This method is shown to be an effective and facile technique for improving the electrochemical performance and stability of nanowire electrodes for applications in Li ion batteries.

  9. 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

  10. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Akbas, Esvet; Gumus, Selcuk; Sumer, Mehmet Rauf; Akyaz, Inci [Yuzuncu Yil University, Van (Turkmenistan); Levent, Abdulkadir [Batman University, Batman (Turkmenistan)

    2010-12-15

    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.

  12. 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.

  13. 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.

  14. 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.

  15. Synthesis and electrochemical characterization of pure and composite cathode materials for solid oxide fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Sun, L.; Favreau-Perreault, M.; Brisard, G. [Universite de Sherbrooke, Departement de Chimie, Sherbrooke, PQ (Canada)

    2004-10-01

    A rare earth cathode composed of various combinations of lanthanum, strontium, copper, iron oxide, cesium and gadolinium oxide was synthesized by using glycine-nitrate combustion techniques, and the Pechini method. Pure and composite complexes composed of these same materials were used to synthesize eight mol per cent yttria-stabilized zirconia cathodes by scanning electron microscopy. Cathode resistances were evaluated by electrochemical impedance spectroscopy and galvanostatic current interruption techniques. Both techniques were found to give identical results in evaluating the total polarization resistance of the cathodes. 24 refs., 2 tabs., 9 figs.

  16. 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.

  17. 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

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. Synthesis and characterization of polyaniline and polyaniline - Carbon nanotubes nanostructures for electrochemical supercapacitors

    Science.gov (United States)

    Bavio, Marcela A.; Acosta, Gerardo G.; Kessler, Teresita

    2014-01-01

    Nanostructures of polyaniline (PANI) and PANI with embedded carbon nanotubes (CNT) were synthesized through a chemical method of self-organization. An oxidative polymerization process was performed in the monomer acid solution with the presence of a surfactant and the addition of multi-walled CNT. The CNT were added with and without pretreatment, CNTf and CNTnf, respectively. Furthermore, ammonium persulfate and sodium dodecyl sulfate were incorporated to the reaction solution as dispersant and oxidizing agents, respectively. Different nanostructures such as nanoparticles or nanotubes were obtained depending on the CNT added, and characterized by scanning electron microscopy, transmission electron microscopy, UV-vis spectroscopy, infrared spectroscopy and electrochemical techniques. Spectroscopy results showed variations in the observed bands of the synthetized nanostructures attributed to changes in the molecular structures, to the state of doped PANI reached during polymerization and to the stabilization of these links by hydrogen bridge interactions. PANI and PANI-CNT composites were evaluated by electrochemical techniques to test their behavior in relation to supercapacitors properties. PANI-CNTf nanocomposites displayed improved capacitive properties in H2SO4 solutions, namely 1744 F g-1at 2 A g-1. Also, the specific capacitance was strongly influenced by the developed morphologies. These characteristics point to their feasible application as supercapacitors materials.

  4. 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.

  5. Synthesis and electrochemical evaluation of an amorphous titanium dioxide derived from a solid state precursor

    Science.gov (United States)

    Joyce, Christopher D.; McIntyre, Toni; Simmons, Sade; LaDuca, Holly; Breitzer, Jonathan G.; Lopez, Carmen M.; Jansen, Andrew N.; Vaughey, J. T.

    Titanium oxides are an important class of lithium-ion battery electrodes owing to their good capacity and stability within the cell environment. Although most Ti(IV) oxides are poor electronic conductors, new methods developed to synthesize nanometer scale primary particles have achieved the higher rate capability needed for modern commercial applications. In this report, the anionic water stable titanium oxalate anion [TiO(C 2O 4) 2] 2- was isolated in high yield as the insoluble DABCO (1,4-diazabicyclo[2.2.2]octane) salt. Powder X-ray diffraction studies show that the titanium dioxide material isolated after annealing in air is initially amorphous, converts to N-doped anatase above 400 °C, then to rutile above 600 °C. Electrochemical studies indicate that the amorphous titanium dioxide phase within a carbon matrix has a stable cycling capacity of ∼350 mAh g -1. On crystallizing at 400 °C to a carbon-coated anatase the capacity drops to 210 mAh g -1, and finally upon carbon burn-off to 50 mAh g -1. Mixtures of the amorphous titanium dioxide and Li 4Ti 5O 12 showed a similar electrochemical profile and capacity to Li 4Ti 5O 12 but with the addition of a sloping region to the end of the discharge curve that could be advantageous for determining state-of-charge in systems using Li 4Ti 5O 12.

  6. 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.

  7. Synthesis, Characterization, Electrochemical and Surface Morphologies of Polyazomethines Containing Silane and Phosphazene Units.

    Science.gov (United States)

    Temizkan, Kevser; Kaya, İsmet

    2017-09-01

    Polyazomethines containing silane and phosphazene groups were synthesized via elimination reactions of dihydroxy compounds containing imine bonding with phosphazane and silane dichloride. The structures of monomers and polymers containing phosphazane and silane groups were supported by 1 H-NMR, 13 C-NMR, FT-IR and UV-Vis techniques. Electrochemical properties of the prepared Schiff bases and polymers were given by cyclic voltammetric (CV) analysis. Thermal properties of synthesized monomers and polymers were determined by TG-DTA and TG-DTA, DMA and DSC techniques, respectively. Molecular mass distributions of polymers are determined with gel permeation chromatography (GPC) measurement. Morphologic images of polymers containing heteroatom (silane/phosphazene) and azomethine linkage in the main chain were investigated by SEM techniques. The electrochemical band gap values of SB-1, SB-2, P-1, P-2 and P-3 compounds were found as 3.09, 3.30, 2.63, 3.07 and 3.04 eV, respectively.

  8. Synthesis and characterization of nanocrystalline vanadium oxide thin films: electrochemical behavior by annealing in different atmosphere

    Science.gov (United States)

    Asiabar, M. Amiri; Mohaghegh, Z.; Ghodsi, F. E.

    2018-01-01

    Nanocrystalline vanadium oxide thin films were prepared using sol-gel dip-coating technique. The effect of heat treatment in different environment including air, N2, Ar, and O2 gas on the structural, optical, electrical, and electrochemical properties of nanocrystalline vanadium oxide thin films were investigated. The results indicated that the calculated average crystallite size was reduced by annealing in Ar environment. Scanning electron microscopy (SEM) images showed layered morphology on the surface of the film annealed in air atmosphere, whereas the film annealed under Ar and N2 ambient revealed granular and wrinkle morphology, respectively. This morphology altered to rather smooth surface by annealing in O2 environment. The optical bandgap of the films were found to be 1.75, 1.84, 2.08, and 2.10 eV annealed in air, O2, N2, and Ar environment, respectively. It was observed that the films annealed under Ar and N2 ambient had low resistivity ( 0.2 Ω cm) and high carrier concentration, while the film annealed in nitrogen environment showed higher mobility of charge carrier. The electrochemical measurements showed that annealing under N2 ambient improved the intercalation of Li ions, leading a higher interfacial capacitance of 19.18 mF Cm-2, and decreased the charge transfer resistance due to surface defects created by heat treatment in nitrogen environment.

  9. Electrochemical Synthesis of Mesoporous CoPt Nanowires for Methanol Oxidation.

    Science.gov (United States)

    Serrà, Albert; Montiel, Manuel; Gómez, Elvira; Vallés, Elisa

    2014-03-28

    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.

  10. 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.

  11. Synthesis and electrochemical properties of Co3O4 nanoparticles by hydrothermal method at different temperatures

    Science.gov (United States)

    Duan, Qiuyan; Chen, Haiyan

    2017-06-01

    In this work, Co3O4 nanoparticles were synthesized by hydrothermal method at different temperatures. The synthesized Co3O4 nanoparticles were characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectrometer (XPS) and nitrogen adsorption-desorption. The Co3O4 nanoparticles prepared at the hydrothermal temperature of 140 °C and at the annealing temperature of 350 °C have a shorter crystal spacing distance associated to the (220) crystal planes, larger BET surface area and more bivalent cobalt on the surface than these of Co3O4 nanoparticles prepared at higher hydrothermal temperature or higher annealing temperature. The supercapacitor performances of synthesized Co3O4 nanoparticles were analysed by cyclic voltammograms (CVs), Galvano static charge/discharge (GCD) and the electrochemical impedance spectroscopy (EIS) in 6 M KOH aqueous electrolyte solution. The Co3O4 nanoparticles produced at lower temperatures exhibit good pseudo capacitance behaviour. Also, owning to the low hydrothermal temperature and the annealing temperature of Co3O4 nanoparticles, they can be relatively low cost in favour of a promising candidate for electrochemical supercapacitors.

  12. Tetradentate Schiff base ligands and their complexes: Synthesis, structural characterization, thermal, electrochemical and alkane oxidation

    Science.gov (United States)

    Ceyhan, Gökhan; Köse, Muhammet; McKee, Vickie; Uruş, Serhan; Gölcü, Ayşegül; Tümer, Mehmet

    Three Schiff base ligands (H2L1-H2L3) with N2O2 donor sites were synthesized by condensation of 1,5-diaminonapthalene with benzaldehyde derivatives. A series of Cu(II), Co(II), Ni(II), Mn(II) and Cr(III) complexes were prepared and characterized by spectroscopic and analytical methods. Thermal, electrochemical and alkane oxidation reactions of the ligands and their metal complexes were investigated. Extensive application of 1D (1H, 13C NMR) and 2D (COSY, HETCOR, HMBC and TOSCY) NMR techniques were used to characterize the structures of the ligands and establish the 1H and 13C resonance assignments of the three ligands. Ligands H2L1 and H2L3 were obtained as single crystals from THF solution and characterized by X-ray diffraction. Both molecules are centrosymmetric and asymmetric unit contains one half of the molecule. Catalytic alkane oxidation reactions with the transition metal complexes investigated using cyclohexane and cyclooctane as substrates. The Cu(II) and Cr(III) complexes showed good catalytic activity in the oxidation of cyclohexane and cyclooctane to desired oxidized products. Electrochemical and thermal properties of the compounds were also investigated.

  13. 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.

  14. 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.

  15. Synthesis and electrochemical detection of a thiazolyl-indole natural product isolated from the nosocomial pathogen Pseudomonas aeruginosa.

    Science.gov (United States)

    Buzid, Alyah; Muimhneacháin, Eoin Ó; Reen, F Jerry; Hayes, Phyllis E; Pardo, Leticia M; Shang, Fengjun; O'Gara, Fergal; Sperry, Jonathan; Luong, John H T; Glennon, Jeremy D; McGlacken, Gerard P

    2016-09-01

    Pseudomonas aeruginosa is a Gram-negative opportunistic pathogen, capable of surviving in a broad range of natural environments and quickly acquiring resistance. It is associated with hospital-acquired infections, particularly in patients with compromised immunity, and is the primary cause of morbidity and mortality in cystic fibrosis (CF) patients. P. aeruginosa is also of nosocomial importance on dairy farms and veterinary hospitals, where it is a key morbidity factor in bovine mastitis. P. aeruginosa uses a cell-cell communication system consisting of signalling molecules to coordinate bacterial secondary metabolites, biofilm formation, and virulence. Simple and sensitive methods for the detection of biomolecules as indicators of P. aeruginosa infection would be of great clinical importance. Here, we report the synthesis of the P. aeruginosa natural product, barakacin, which was recently isolated from the bovine ruminal strain ZIO. A simple and sensitive electrochemical method was used for barakacin detection using a boron-doped diamond (BDD) and glassy carbon (GC) electrodes, based on cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The influence of electrolyte pH on the peak potential and peak currents was also investigated. At pH 2.0, the peak current was linearly dependent on barakacin concentration (in the range used, 1-10 μM), with correlation coefficients greater than 0.98 on both electrodes. The detection limit (S/N = 3) on the BDD electrode was 100-fold lower than that obtained on the GC electrode. The optimized method using the BDD electrode was extended to bovine (cow feces) and human (sputum of a CF patient) samples. Spiked barakacin was easily detected in these matrices at a limit of 0.5 and 0.05 μM, respectively. Graphical abstract Electrochemical detection of barakacin.

  16. 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.

  17. Synthesis, electrochemical, structural and theoretical study of new derivatives of OABAN and OABAO heterocycles

    Czech Academy of Sciences Publication Activity Database

    Mikysek, T.; Kvapilová, Hana; Doušová, H.; Josefík, F.; Šimůnek, P.; Růžičková, Z.; Ludvík, Jiří

    2017-01-01

    Roč. 455, č. 2 (2017), s. 465-472 ISSN 0020-1693 R&D Projects: GA MŠk LD14129 Institutional support: RVO:61388955 Keywords : boron heterocycles * synthesis * electrochemistry Subject RIV: CG - Electrochemistry OBOR OECD: Electrochemistry (dry cells, batteries, fuel cells, corrosion metals, electrolysis) Impact factor: 2.002, year: 2016

  18. Corrigendum to "Synthesis, crystal structure and electrochemical and DNA binding studies of oxygen bridged-copper(II) carboxylate" [J. Mol. Struct. 1093 (2015) 135-143

    Science.gov (United States)

    Iqbal, Muhammad; Ali, Saqib; Tahir, Muhammad Nawaz; Muhammad, Niaz; Shah, Naseer Ali; Sohail, Manzar; Pandarinathan, Vedapriya

    2017-04-01

    The authors regret to inform that Scheme 1 in the article titled 'Synthesis, crystal structure and electrochemical and DNA binding studies of oxygen bridged-copper(II) carboxylate' in vol. 1093 of the Journal of Molecular Structure is incorrect. The corrected scheme is as shown in this correction. This is purely a copy error. The error does not affect the conclusion in paper. The authors would like to apologize for any inconvenience caused.

  19. Electrochemical synthesis and characterization of hierarchically branched ZnO nanostructures on ensembles of gold nanowires

    International Nuclear Information System (INIS)

    Ongaro, Michael; Gambirasi, Arianna; Favaro, Monica; Ugo, Paolo

    2012-01-01

    Highlights: ► ZnO branched nanofibres for photoelectrochemical applications. ► Branched nanostructures are obtained by electrochemical deposition of ZnO on gold template nanowires. ► Branched nanowires crystallographic phase determined by electron back scatter diffraction. ► Branched structures display improved performances for the photoelectrochemical oxidation of water. - Abstract: This study presents an electrosynthetic methodology to obtain hierarchically structured ZnO electrodes with improved surface area, by exploiting gold nanowires ensembles (3D-NEEs) as the growing substrate. By this way, semiconductor electrodes organized in the shape of fir-like branches are obtained. Branched nanofibres are characterized by electron microscopy and electron backscatter diffraction (EBSD), the latter technique allowing the determination of the crystalline habit of individual nanostructures. The hierarchical branched nanowires show enhanced performances with respect to water photooxidation in comparison with already known nanostructured materials such as 1D-ZnO nanowires.

  20. Additive-mediated electrochemical synthesis of platelike copper crystals for methanol electrooxidation.

    Science.gov (United States)

    Venkatasubramanian, Rajesh; He, Jibao; Johnson, Michael W; Stern, Ilan; Kim, Dae Ho; Pesika, Noshir S

    2013-10-29

    A room-temperature electrochemical approach to synthesizing anisotropic platelike copper microcrystals and nanocrystals in the presence of potassium bromide is presented. Morphological and elemental characterization was performed using SEM, TEM, and XRD to confirm the anisotropic morphology and crystal structure of the synthesized copper particles. A possible mechanism for explaining the anisotropic crystal growth is proposed on the basis of the preferential adsorption of bromide ions to selective crystal faces. The shape-dependent electrocatalytic property of copper particles is demonstrated by its enhanced catalytic activity for methanol oxidation. Further development of such anisotropic copper particles localized on an electrode surface will lead us to find a suitable alternative for noble metal-based electrocatalysts for the methanol oxidation reaction relevant to fuel cells.

  1. Electrochemical synthesis of birnessite-type layered manganese oxides for rechargeable lithium batteries

    Science.gov (United States)

    Nakayama, Masaharu; Kanaya, Taku; Lee, Jong-Won; Popov, Branko N.

    Layered manganese dioxide (MnO 2) films intercalated with Li +, Na + or Mg 2+ ions were synthesized by a one-step electrochemical method. The electrodeposition was potentiostatically performed by applying an anodic potential of 1.0 V vs. Ag/AgCl in an aqueous MnSO 4 solution containing a perchlorate salt of the cation. The electrodeposited oxide films have a birnessite-type layered structure with alkali cations and water molecules between manganese oxide layers. The galvanostatic charge-discharge experiments performed in 1 M LiPF 6-DME/PC solution indicated that the Mg 2+-intercalated MnO 2 electrode exhibits an initial discharge capacity as large as 140 mAh g -1 and it shows a better capacity retention during cycling as compared with the Li +- or Na +-intercalated MnO 2 electrode.

  2. Clean and Green Synthesis of New Benzothiazole Derivatives via Electrochemical Oxidation of Catechol Derivatives

    Directory of Open Access Journals (Sweden)

    Mansour Arab Chamjangali

    2016-06-01

    Full Text Available Electrochemical oxidation of the catechols 1a and 1b is studied in the presence of 6-methyl-2-thouracil (3b and 6-propyl-2-thiouracil (3a as nucleophiles in a phosphate buffer (0.15 mol L−1, pH = 6.8/DMF (95:5 solution using cyclic voltammetry and controlled-potential coulometry. The results obtained indicate that the quinones derived from the catechols participate in 1,4-Michael-addition reactions with the nucleophiles to form the corresponding new benzothiazole compounds. In this work, we derive a variety of products with good yields using controlled potential at graphite electrodes in an undivided cell. This work is licensed under a Creative Commons Attribution 4.0 International License.

  3. The Challenge of Electrochemical Ammonia Synthesis: A New Perspective on the Role of Nitrogen Scaling Relations.

    Science.gov (United States)

    Montoya, Joseph H; Tsai, Charlie; Vojvodic, Aleksandra; Nørskov, Jens K

    2015-07-08

    The electrochemical production of NH3 under ambient conditions represents an attractive prospect for sustainable agriculture, but electrocatalysts that selectively reduce N2 to NH3 remain elusive. In this work, we present insights from DFT calculations that describe limitations on the low-temperature electrocatalytic production of NH3 from N2 . In particular, we highlight the linear scaling relations of the adsorption energies of intermediates that can be used to model the overpotential requirements in this process. By using a two-variable description of the theoretical overpotential, we identify fundamental limitations on N2 reduction analogous to those present in processes such as oxygen evolution. Using these trends, we propose new strategies for catalyst design that may help guide the search for an electrocatalyst that can achieve selective N2 reduction. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Novel Mannich bases bearing pyrazolone moiety. Synthesis, characterization and electrochemical studies

    Directory of Open Access Journals (Sweden)

    KRISHNA NAIK

    2013-04-01

    Full Text Available The present investigation describes a series of new {4-[3-Methyl-5-oxo-4-(4|-substituted phenyl hydrazono-4,5-dihydro-pyrazol-1-yl]-phenoxy}-acetic acid (2-oxo-1-piperidine-1-ylmethyl-1,2-dihydro–indol-3-ylidene-hydrazides synthesized by the Mannich reaction of {4-[3-Methyl-5-oxo-4-(4|-substituted phenyl hydrazono-4,5-dihydro-pyrazol-1-yl]-phenoxy}-acetic acid (2-oxo-1,2-dihydro-indol-3-ylidene-hydrazide with aqueous formaldehyde and a solution of piperidine in dimethylformamide. These novel Mannich bases were characterized by elemental analysis, IR, 1H NMR and mass spectral data. Electrochemical behavior of these compounds were studied by two techniques namely polarography and cyclic voltammetry. The results from both the techniques were compared and the reduction mechanism in acidic as well as basic medium was proposed.

  5. Synthesis of nanosized vanadium pentoxide/carbon composites by spray pyrolysis for electrochemical capacitor application

    International Nuclear Information System (INIS)

    Wang Bei; Konstantinov, Konstantin; Wexler, David; Liu Hao; Wang Guoxiu

    2009-01-01

    Nanostructured vanadium pentoxide/carbon (V 2 O 5 /carbon) composite powders with enhanced specific capacitance were synthesized by the spray pyrolysis technique. Electrochemical properties were examined by the cyclic voltammetry technique. Following analysis of powders sprayed at different temperatures, composite powders obtained at an optimum temperature of 450 deg. C yielded a maximum specific capacitance of 295 F g -1 in 2 M KCl electrolyte at a 5-mV s -1 scan rate. The weight percentage of carbon-related species was 2.7 wt% in this V 2 O 5 /carbon composite, as detected by thermogravimetric analysis (TGA) and confirmed by transmission electron microscope energy dispersive spectroscopy (TEM-EDS) analysis. Following initial X-ray diffraction (XRD) characterization, scanning electron microscope (SEM), TEM and high-resolution TEM (HRTEM) imaging revealed a specific morphology of spherical shell agglomerates of V 2 O 5 nanorods and nanoribbons, with each shell comprising a network of these one- and two-dimensional nanoparticles in an amorphous carbon matrix. The V 2 O 5 network was not fully dense, and the majority of the nanorod sizes were in the range of 50-150 nm, with additional long nanoribbons extending from the outsides of the spherical shells. The specific surface area was 18 m 2 g -1 for the composite powders, and the pore size distribution revealed that the majority of pores had diameters in the range of 40-50 A, which was relatively larger than the pore diameters obtained at 500 deg. C and would be beneficial for electrochemical performance. The enhancement of the specific capacitance in V 2 O 5 /carbon composites was attributed to the distribution of amorphous carbon throughout the V 2 O 5 and the particular open nanostructure

  6. 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.

  7. Synthesis of NiS-Graphene Nanocomposites and its Electrochemical Performance for Supercapacitors

    Science.gov (United States)

    Pandey, Chandan Abhishek; Ravuri, Syamsai; Ramachandran, R.; Santhosh, R.; Ghosh, Sourav; Sitaraman, S. R.; Grace, Andrews Nirmala

    The aim of this work is to synthesize nickel sulfide-graphene (NiS/G) nanocomposites with different compositions and to analyze the structural and electrochemical capacity and compatibility for their application as supercapacitor material with enhanced charge storage capacity and reduced impedance. NiS nanoparticles (NPs) loaded on graphene were synthesized at various concentrations of graphene by a simple hydrothermal route from nickel sulphate and graphene oxide as precursors in the presence of PVP as surfactant and thioacetamide (TAA) as sulfur source. The composites structural, morphological and physical properties were analyzed by X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), Energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy (XPS) and Fourier Transform-infrared (FT-IR) analysis. SEM measurements showed the presence of surface attachment of the NiS NPs onto the graphene sheets. To assess the properties of the nanocomposites for their applicability in supercapacitors, electrochemical analysis was carried out in 6M KOH electrolyte. Three different samples with different graphene contents — GNiS-10 with 10 wt.%, GNiS-20 with 20 wt.% and GNiS-40 with 40 wt.% were prepared. The specific capacitances obtained for the nanocomposites were calculated to be 84.33F/g, 129.66F/g, 187.53F/g at 10mV/s scan rate, respectively. The EIS data showed that the loading of NiS NPs on graphene caused the reduction in impedance at high frequency and has a long cycle life (over 1000 cycles).

  8. 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.

  9. 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.

  10. Single transition metal atom embedded into a MoS2nanosheet as a promising catalyst for electrochemical ammonia synthesis.

    Science.gov (United States)

    Zhao, Jia; Zhao, Jingxiang; Cai, Qinghai

    2018-03-21

    The electrochemical reduction of N2 to NH3 (NRR) under ambient conditions is significant for sustainable agriculture. Here, by means of density functional theory (DFT) computations, the potential of a series of single transition metal (TM) atoms embedded into a MoS2 monolayer with an S-vacancy (TM/MoS2) as electrocatalysts for NRR was systematically investigated. Our DFT results revealed that among all these considered candidate catalysts, the single Mo atom embedded into the MoS2 nanosheet was found to be the most active catalyst for NRR with an onset potential of -0.53 V, in which the hydrogenation of the adsorbed N2* to N2H* is the potential-determining step. The high stabilization of the N2H* species is responsible for the superior performance of the embedded Mo atom for the NRR, which is well consistent with its d-band center. Our findings may facilitate the further design of single-atom electrocatalysts with high efficiency for NH3 synthesis at room temperature.

  11. 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.

  12. 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.

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

    Science.gov (United States)

    Khalil, Ibrahim; Julkapli, Nurhidayatullaili Muhd; Yehye, Wageeh A.; Basirun, Wan Jefrey; Bhargava, Suresh K.

    2016-01-01

    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. PMID:28773528

  14. Simple route to anchor silver nanoparticles into thiol-functionalized mesoporous silica: synthesis, characterization and electrochemical applications

    Energy Technology Data Exchange (ETDEWEB)

    Sonkar, Piyush Kumar; Ganesan, Vellaichamy, E-mail: velganesh@yahoo.com, E-mail: velgan@bhu.ac.in; Gupta, Rupali; Yadav, Dharmendra Kumar [Banaras Hindu University, Department of Chemistry, Institute of Science (India)

    2016-10-15

    This work describes an elegant route to synthesize silver nanoparticles (AgNPs) into thiol-functionalized mesoporous silica (TFS). The successful synthesis of AgNPs in TFS (Ag-TFS) is confirmed by spectroscopy and microscopy techniques. TEM images reveal the presence of distorted spherical shapes of AgNPs with 1–30 nm size in the TFS. Though the distribution of AgNPs is uniform throughout the TFS spheres, the size of the AgNPs varies. The electrocatalytic activity of Ag-TFS on the oxidation of nitrite is studied, and its determination is compared with the TFS based on differential pulse voltammetry (DPV). The Ag-TFS-coated glassy carbon (GC) electrode (GC/Ag-TFS) shows stable and superior electrochemical features for nitrite oxidation over the GC/TFS electrode as studied by DPV. The linear calibration range for nitrite determination at GC/Ag-TFS is found to be 1.0 µM–20.0 mM with a sensitivity of 73 µAmM{sup −1} cm{sup −2} and a detection limit of 0.5 µM.Graphical Abstract.

  15. Synthesis and Electrochemical Properties of Two-Dimensional RGO/Ti3C2Tx Nanocomposites

    Directory of Open Access Journals (Sweden)

    Changjie Shen

    2018-01-01

    Full Text Available MXene is a new type of two-dimensional layered material. Herein, a GO/Ti3C2Tx nanocomposite was prepared by a simple liquid phase method, and the obtained GO/Ti3C2Tx was transformed into RGO/Ti3C2Tx under high temperature with Ar/H2. The prepared samples were characterized using X-ray diffraction (XRD, Raman measurement, scanning electron microscopy (SEM, energy disperse spectroscopy (EDS, and X-ray photoelectron spectroscopy (XPS. As an electrode material in lithium-ion batteries, the RGO/Ti3C2Tx nanocomposite exhibited an excellent electrochemical performance and an excellent rate performance. Compared to pure Ti3C2Tx, the nanocomposite had a better reversible capacity at different current densities and had no attenuation after 200 cycles, which is one time higher than pure Ti3C2Tx. The improvement in the specific capacity was due to the excellent electrical conductivity and the unique structure of RGO, in which a charge transfer bridge was built among the Ti3C2Tx flakes. Such a bridge shortened the transmission distance of the electrons and ions and effectively controlled the restacking of the laminated materials.

  16. Electrochemical zinc insertion into W18O49: Synthesis and characterization of new bronzes

    International Nuclear Information System (INIS)

    Martinez-de la Cruz, A.; Amador, U.; Rodriguez-Carvajal, J.; Garcia-Alvarado, F.

    2005-01-01

    Divalent zinc ions have been electrochemically inserted into W 18 O 49 , producing zinc bronzes. Under our experimental conditions, W 18 O 49 accepts zinc reversibly as a guest up to 0.9 ions per formula. The reaction seems to proceed through the formation of a solid solution in which the W-O framework of the parent oxide is maintained. The location of the Zn 2+ ions in the framework of W 18 O 49 has been determined by neutron diffraction on a chemically prepared sample having the composition Zn 0.34 W 18 O 49 . As a main result, we found that Zn prefers to insert in one of the four types of quadrangular tunnels. More precisely, it is displaced from the center to occupy a low coordination site. This result indicates that a significant covalent character exists in the Zn-O bond. - Graphical Abstract: The structure of Zn 0.36 W 18 O 49 projected along the b-axis

  17. Synthesis, characterization, anticancer activity, thermal and electrochemical studies of some novel uranyl Schiff base complexes

    Energy Technology Data Exchange (ETDEWEB)

    Asadi, Zahra; Asadi, Mozaffar; Firuzabadi, Fahimeh Dehghani [Shiraz Univ. (Iran, Islamic Republic of). Dept. of Chemistry; Yousefi, Reza; Jamshidi, Mehrnaz [Shiraz Univ. (Iran, Islamic Republic of). Protein Chemistry Lab. (PCL)

    2014-04-15

    Some tetradentate N{sub 2}O{sub 2} Schiff base ligands, such as N,N{sup '}-bis(naphtalidene)-1,2-phenylenediamine, N,N{sup '}-bis(naphtalidene)-4-methyl-1,2-phenylenediamine, N,N{sup '}-bis(naphtalidene)-4-chloro-1,2-phenylenediamine, N,N{sup '}-bis(naphtalidene)-4-nitro-1,2-phenylenediamine, N,N{sup '}-bis(naphtalidene)-4-carboxyl-1,2-phenylenediamine, and their uranyl complexes were synthesized and characterized by {sup 1}H NMR, IR, UV-Vis spectroscopy, TG (thermogravimetry), and elemental analysis (C.H.N.). Thermogravimetric analysis shows that uranyl complexes have very different thermal stabilities. This method is used also to establish that only one solvent molecule is coordinated to the central uranium ion and this solvent molecule does not coordinate strongly and is removed easier than the tetradentate ligand and also trans oxides. The electrochemical properties of the uranyl complexes were investigated by cyclic voltammetry. Electrochemistry of these complexes showed a quasireversible redox reaction without any successive reactions. Also, the kinetic parameters of thermal decomposition were calculated using Coats-Redfern equation. According to Coats-Redfern plots the kinetics of thermal decomposition of the studied complexes is first-order in all stages. Anticancer activity of the uranyl Schiff base complexes against cancer cell lines (Jurkat) was studied and determined by MTT (3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyltetrazoliumbromide) assay.

  18. Synthesis and Characterization of Novel Polythiophenes Containing Pyrene Chromophores: Thermal, Optical and Electrochemical Properties.

    Science.gov (United States)

    Valderrama-García, Bianca X; Rodríguez-Alba, Efraín; Morales-Espinoza, Eric G; Moineau Chane-Ching, Kathleen; Rivera, Ernesto

    2016-01-30

    A novel series of pyrene containing thiophene monomers TPM1-5 were synthesized and fully characterized by FTIR, MS, ¹H- and (13)C-NMR spectroscopy; their thermal properties were determined by TGA and DSC. These monomers were chemically polymerized using FeCl3 as oxidizing agent to give the corresponding oligomers TPO1-5) and they were electrochemically polymerized to obtain the corresponding polymer films deposited onto ITO. All oligomers exhibited good thermal stability, with T10 values between 255 and 299 °C, and Tg values varying from 36 to 39 °C. The monomers showed an absorption band at 345 nm due to the S0 → S2 transition of the pyrene group, whereas the fluorescence spectra showed a broad emission band arising from the "monomer" emission at 375-420 nm. The obtained polymers exhibited two absorption bands at 244 and 354 nm, due to the polythiophene and the pyrene moieties, respectively. The fluorescence spectra of polymers showed a broad "monomer" emission at 380-420 nm followed by an intense excimer emission band at 570 nm, due to the presence of intramolecular pyrene-pyrene interactions in these compounds.

  19. Synthesis and Electrochemical Performance of a Lithium Titanium Phosphate Anode for Aqueous Lithium-Ion Batteries

    KAUST Repository

    Wessells, Colin

    2011-01-01

    Lithium-ion batteries that use aqueous electrolytes offer safety and cost advantages when compared to today\\'s commercial cells that use organic electrolytes. The equilibrium reaction potential of lithium titanium phosphate is -0.5 V with respect to the standard hydrogen electrode, which makes this material attractive for use as a negative electrode in aqueous electrolytes. This material was synthesized using a Pechini type method. Galvanostatic cycling of the resulting lithium titanium phosphate showed an initial discharge capacity of 115 mAh/g and quite good capacity retention during cycling, 84% after 100 cycles, and 70% after 160 cycles at a 1 C cycling rate in an organic electrolyte. An initial discharge capacity of 113 mAh/g and capacity retention of 89% after 100 cycles with a coulombic efficiency above 98% was observed at a C/5 rate in pH -neutral 2 M Li2 S O4. The good cycle life and high efficiency in an aqueous electrolyte demonstrate that lithium titanium phosphate is an excellent candidate negative electrode material for use in aqueous lithium-ion batteries. © 2011 The Electrochemical Society.

  20. Synthesis and Electrochemical Analyses of Manganese Oxides for Super-Capacitors.

    Science.gov (United States)

    Kim, Taewoo; Hwang, Hyein; Jang, Jaeyong; Park, Inyeong; Shim, Sang Eun; Baeck, Sung-Hyeon

    2015-11-01

    δ-Phase and α-phase manganese oxides were prepared using a hydrothermal method and their electrochemical properties were characterized. The influence of calcination temperature on the properties of manganese oxides was studied. Crystallinities were studied by X-ray diffraction, and scanning and transmission electron microscopy were utilized to examine morphologies. Average pore sizes and specific surface areas of samples were analyzed using the Barret-Joyner-Halenda and Brunauer-Emmett-Teller methods, respectively. After calcination in the range 300 degrees C to 600 degrees C, changes in morphology and crystallinity were observed. The flower-like shape of as synthesized samples became nanorod-like and the δ-phase changed to the α-phase. These changes may have been due to the removal of water during calcination. Furthermore, a transition stage in which the two phases coexisted was observed. Synthesized manganese oxides were mixed with carbon by sonification, to increase electric conductivity and to induce a synergistic effect between pseudo-capacitor and electric double layer capacitor (EDLC). Specific capacitances and rate durability of each composite were investigated by cyclic voltammetry in 1 M Na2SO4 electrolyte at different scan rates. MnO2 calcined at 400 degrees C exhibited the highest capacitance, probably due to its high surface area and more porous structure.

  1. Electrochemical Synthesis of Ordered Titania Nanotubes in Mixture of Ethylene Glycol and Glycerol Electrolyte

    International Nuclear Information System (INIS)

    Chin, L.Y.; Zulkarnain Zainal; Zuraida Khusaimi; Siti Sarah Ismail

    2016-01-01

    The electrolyte chemistry (nature and its composition) plays a critical role in determining the nano tube architecture and its growth process. In the present study, the formation of well-ordered titania nano tubes (TNT) is achieved by electrochemical anodization of titanium substrate in aqueous ethylene glycol-glycerol electrolyte (EG/Gly). The resulted samples were characterized using X-ray Diffraction (XRD) and the morphology changes were monitored by Field Emission Scanning Electron Microscopy (FESEM). Compositional changes of the titania nano tubes (TNT) were determined using Energy Dispersive X-ray Spectroscopy (EDX). The influence of anodization voltage, volume ratio of electrolyte and NH 4 F content on the morphology and geometry of titania nano tubes have been investigated. The nature of electrolytes influenced the ordering and uniformity of nano tubes. In addition, nano tubes with various diameters ranging from 62 - 112 nm and lengths of 1.1 - 1.3 μm were obtained by controlling the anodization voltage and volume ratio of EG/ Gly. Ultimately, anodization of Ti at 20 V in 1:1 volume ratio of EG/ Gly containing 0.25 - 1.0 wt.% NH 4 F appears to be an optimum condition for controlling the ordering of nano tubes. (author)

  2. Synthesis, exploration of energy storage and electrochemical sensing properties of hematite nanoparticles

    International Nuclear Information System (INIS)

    Ramasami, Alamelu K.; Ravishankar, T.N.; Sureshkumar, K.; Reddy, M.V.; Chowdari, B.V.R.; Ramakrishnappa, T.; Balakrishna, Geetha R.

    2016-01-01

    Gel-combustion, solution combustion and molten salt methods were used to synthesize hematite nanoparicles. Two weight ratios of precursor (Ferric nitrate) to fuel (Cassava Starch) (1:0.5, 1:1) were used in gel-combustion technique. Ferric nitrate as a precursor and ethylenediamine tetraacetic acid as fuel (in stoichiometric proportions) were used in the solution combustion method. Ferric oxalate was the precursor in molten salt method. The structural parameters of the hematite nanoparticles were studied by X-ray diffraction. The optical properties, including band gap studies were done by UV–Visible spectroscopy. The morphological studies were carried out by Scanning Electron Microscope. The energy storage capacity of the molten salt method-hematite nanoparticles surpassed (920 mAhg −1 ) the others while the equal-weight- ratio-hematite nanoparticles synthesized by gel-combustion method exhibited better dopamine sensor properties. - Highlights: • Hematite nanoparticles were synthesized by gel, solution combustion and molten salt methods. • Gel-combustion involved the use of natural fuel extracted from the root tubers of Manihot esculenta. • Two ratios of fuel to precursors were attempted in gel combustion method. • The product formed from the equal weight ratio of fuel to precursor was a very good electrochemical dopamine sensor. • The product formed by molten salt method exhibited good battery behaviour (Li-ion battery).

  3. Synthesis and Characterization of Novel Polythiophenes Containing Pyrene Chromophores: Thermal, Optical and Electrochemical Properties

    Directory of Open Access Journals (Sweden)

    Bianca X. Valderrama-García

    2016-01-01

    Full Text Available A novel series of pyrene containing thiophene monomers TPM1–5 were synthesized and fully characterized by FTIR, MS, 1H- and 13C-NMR spectroscopy; their thermal properties were determined by TGA and DSC. These monomers were chemically polymerized using FeCl3 as oxidizing agent to give the corresponding oligomers TPO1–5 and they were electrochemically polymerized to obtain the corresponding polymer films deposited onto ITO. All oligomers exhibited good thermal stability, with T10 values between 255 and 299 °C, and Tg values varying from 36 to 39 °C. The monomers showed an absorption band at 345 nm due to the S0 → S2 transition of the pyrene group, whereas the fluorescence spectra showed a broad emission band arising from the “monomer” emission at 375–420 nm. The obtained polymers exhibited two absorption bands at 244 and 354 nm, due to the polythiophene and the pyrene moieties, respectively. The fluorescence spectra of polymers showed a broad “monomer” emission at 380–420 nm followed by an intense excimer emission band at 570 nm, due to the presence of intramolecular pyrene-pyrene interactions in these compounds.

  4. Facile Green Synthesis of BCN Nanosheets as High-Performance Electrode Material for Electrochemical Energy Storage.

    Science.gov (United States)

    Karbhal, Indrapal; Devarapalli, Rami Reddy; Debgupta, Joyashish; Pillai, Vijayamohanan K; Ajayan, Pulickel M; Shelke, Manjusha V

    2016-05-17

    Two-dimensional hexagonal boron carbon nitride (BCN) nanosheets (NSs) were synthesized by new approach in which a mixture of glucose and an adduct of boric acid (H3 BO3 ) and urea (NH2 CONH2 ) is heated at 900 °C. The method is green, scalable and gives a high yield of BCN NSs with average size of about 1 μm and thickness of about 13 nm. Structural characterization of the as-synthesized material was carried out by several techniques, and its energy-storage properties were evaluated electrochemically. The material showed excellent capacitive behaviour with a specific capacitance as high as 244 F g(-1) at a current density of 1 A g(-1) . The material retains up to 96 % of its initial capacity after 3000 cycles at a current density of 5 A g(-1) . © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Synthesis, exploration of energy storage and electrochemical sensing properties of hematite nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Ramasami, Alamelu K. [Centre for Nano and Material Sciences, Jain University, Bangalore 562112 (India); Department of Physics, Advanced Batteries Lab, National University of Singapore, 117542 (Singapore); Ravishankar, T.N.; Sureshkumar, K. [Centre for Nano and Material Sciences, Jain University, Bangalore 562112 (India); Reddy, M.V.; Chowdari, B.V.R. [Department of Physics, Advanced Batteries Lab, National University of Singapore, 117542 (Singapore); Ramakrishnappa, T. [Centre for Nano and Material Sciences, Jain University, Bangalore 562112 (India); Balakrishna, Geetha R., E-mail: br.geetha@jainuniversity.ac.in [Centre for Nano and Material Sciences, Jain University, Bangalore 562112 (India)

    2016-06-25

    Gel-combustion, solution combustion and molten salt methods were used to synthesize hematite nanoparicles. Two weight ratios of precursor (Ferric nitrate) to fuel (Cassava Starch) (1:0.5, 1:1) were used in gel-combustion technique. Ferric nitrate as a precursor and ethylenediamine tetraacetic acid as fuel (in stoichiometric proportions) were used in the solution combustion method. Ferric oxalate was the precursor in molten salt method. The structural parameters of the hematite nanoparticles were studied by X-ray diffraction. The optical properties, including band gap studies were done by UV–Visible spectroscopy. The morphological studies were carried out by Scanning Electron Microscope. The energy storage capacity of the molten salt method-hematite nanoparticles surpassed (920 mAhg{sup −1}) the others while the equal-weight- ratio-hematite nanoparticles synthesized by gel-combustion method exhibited better dopamine sensor properties. - Highlights: • Hematite nanoparticles were synthesized by gel, solution combustion and molten salt methods. • Gel-combustion involved the use of natural fuel extracted from the root tubers of Manihot esculenta. • Two ratios of fuel to precursors were attempted in gel combustion method. • The product formed from the equal weight ratio of fuel to precursor was a very good electrochemical dopamine sensor. • The product formed by molten salt method exhibited good battery behaviour (Li-ion battery).

  6. 6-Aminocoumarin-naphthoquinone conjugates: design, synthesis, photophysical and electrochemical properties and DFT calculations

    Energy Technology Data Exchange (ETDEWEB)

    Miranda, Fabio S.; Ronconi, Celia M.; Sousa, Mikaelly O.B.; Silveira, Gleiciani Q.; Vargas, Maria D., E-mail: miranda@vm.uff.br, E-mail: mdvargascp@gmail.com [Universidade Federal Fluminense (UFF), Niteroi, RJ (Brazil). Inst. de Quimica

    2014-01-15

    Four novel 6-aminocoumarin-naphthoquinone conjugates were synthesized and their photophysical and electrochemical properties, investigated. 2-Chloro-3-(2-oxo-2H-chromen-6- ylamino)-1,4-naphthoquinone 1 did not present appreciable fluorescence in solution in comparison with 6-aminocoumarin, 6-AC. In order to understand the reasons for the fluorescence quenching in this compound, two strategies were attempted. Firstly, compound 1 was N-methylated to remove the intramolecular N-H...O=C electrostatic interaction that maintained the two units fixed, but the emission properties of the product 2 were not significantly different from those of 1. Time-dependent density functional theory (TD-DFT) calculations of compounds 1 and 2 indicate that the fluorescence quenching is related to the electron acceptor character of the naphthoquinone ring. The second strategy, therefore, involved the substitution of the chlorine atom in position 2 of the naphthoquinone nucleus for different electron donor groups (compounds 3-5), but again the emission properties did not change significantly. To explain these experimental findings, TD-DFT calculations of the ground (S{sub 0}) and excited (S{sub 1}) states of all molecules in solution were carried out. The results suggest that the energy states in these conjugates are such that the fluorescent group (6-AC) donates electrons to the naphthoquinone LUMO resulting in an oxidative photoinduced electron transfer (oxidative-PET). (author)

  7. Electrochemical synthesis and impedance characterization of nano-patterned biosensor substrate.

    Science.gov (United States)

    Takhistov, Paul

    2004-06-15

    The nano-porous anodic aluminum oxide has been used as a substrate material for enzymatic biosensor operating in aqueous solutions. Nano-scale porous structure was formed by electrical anodization in an acid solution. By changing anodization conditions, such as electrolyte concentration, temperature, and anodization time, the ordered hexagonal porous structure with well-controlled pore size and depth can be obtained. Nano-porous alumina substrate with adsorbed enzymes was used as an enzyme electrode and pH sensor. The pH changes are driven by the enzymatic reactions, e.g. penicillin G hydrolysis to form penicilloic acid in the presence of penicillinaze. The advantage of physical adsorption used to bound penicillinaze, the model enzyme in this work, to the porous structure, is that usually no reagents are required and only a minimum of "activation" or clean-up steps. Adsorption tends to be less disruptive to enzyme proteins than chemical attachment. Due to the increased active sensor area, the immobilization of enzymes has been enhanced, which in turn improved the electrode's sensitivity. To characterize the interactions of enzymes with nano-porous alumina oxide, electrochemical impedance spectroscopy (EIS) was used.

  8. 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.

  9. Synthesis and Electrochemical Studies of ReO3 Type Phase Nb3O7F

    Directory of Open Access Journals (Sweden)

    D. Saritha

    2018-04-01

    Full Text Available In latest era, explore for alternative materials to carbonaceous negative electrodes working at higher potential in lithium ion batteries is given enormous significance to avoid lithium plating and electrolyte decomposition. Niobium based oxides show enhanced results as choice to carbonaceous anodes and also Nb5+/4+ redox couple working at approximately 1.5V vs. lithium.The redox potential of the niobium metal ion (~1.5V and the structure of Nb3O7F encourage us lithium insertion studies. Nb3O7F compound has been synthesized through a simple solid state method to explore as anode material. A structural and electrochemical property of this compound is studied in detail.The charge-discharge curves are obtained galvanostatically at C/5 rate. In first discharge step, 5.3 Li can be inserted into four step process between 3.0 – 1.0 V with a specific capacity of 350 mAhg-1. Four plateaus are observed at 1.65, 1.3,1.2 and 1.1V. During charge 1.3 Li can be extracted with an irreversible capacity loss. The total first-charge capacity is 86 mAhg-1 corresponding to the extraction of 1.3 Li. These cells show a reversible capacity 86 mAhg-1 after 25 cycles. The detailed results will be described and discussed.

  10. Highly Soluble Monoamino-Substituted Perylene Tetracarboxylic Dianhydrides: Synthesis, Optical and Electrochemical Properties

    Directory of Open Access Journals (Sweden)

    Kew-Yu Chen

    2014-12-01

    Full Text Available Three dialkylamino-substituted perylene tetracarboxylic dianhydrides with different n-alkyl chain lengths (n = 6, 12 or 18, 1a–1c, were synthesized under mild conditions in high yields and were characterized by 1H NMR, 13C NMR and high resolution mass spectroscopy. Their optical and electrochemical properties were measured using UV-Vis and emission spectroscopic techniques, as well as cyclic voltammetry (CV. This is the first time that the structures and the properties of monoamino-substituted perylene tetracarboxylic dianhydrides have been reported. These molecules show a deep green color in both solution and the solid state and are soluble in most organic solvents. They all show a unique charge transfer emission in the near-infrared region, and the associated peaks exhibit solvatochromism. The dipole moments of the compounds have been estimated using the Lippert-Mataga equation, and upon excitation, they show slightly larger dipole moment changes than those of corresponding perylene diimides, 2a–2c. Additionally, Compounds 1a–1c undergo two quasi-reversible one-electron oxidations and two quasi-reversible one-electron reductions in dichloromethane at modest potentials. Complementary density functional theory calculations performed on these chromophores are reported in order to gain more insight into their molecular structures and optical properties.

  11. 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.

  12. Synthesis, crystal structure and electrochemical and DNA binding studies of oxygen bridged-copper(II) carboxylate

    Science.gov (United States)

    Iqbal, Muhammad; Ali, Saqib; Tahir, Muhammad Nawaz; Muhammad, Niaz; Shah, Naseer Ali; Sohail, Manzar; Pandarinathan, Vedapriya

    2015-08-01

    A new binuclear O-bridged Cu(II) complex with 4-chlorophenyl acetate and 2,2‧-bipyridine has been synthesized and characterized using FT-IR, powder and single crystal XRD and electrochemical solution studies. The results revealed that the two penta-coordinated Cu(II) centers are linked by two carboxylate ligands in end-on bonding fashion. The coordination geometry is slightly distorted square pyramidal (SP) with bridging oxygen atoms occupying the apical position and other ligands lying in the equatorial plane. The striking difference in Cu-O bond distance of the bridging oxygen atom in the complex may be responsible for the SP geometry of Cu(II) ion. The complex gave rise to metal centered irreversible electro-activity where one electron Cu(II)/Cu(III) oxidation process and a single step two electron Cu(II)/Cu(0) reduction process was observed. The redox processes were found predominantly adsorption controlled. The values of diffusion coefficient and heterogeneous rate constant for oxidation process were 6.98 × 10-7 cm2 s-1 and 4.60 × 10-5 cm s-1 while the corresponding values for reduction were 5.30 × 10-8 cm2 s-1 and 5.41 × 10-6 cm s-1, respectively. The formal potential and charge transfer coefficient were also calculated. The DNA-binding ability was explored through cyclic voltammetry and UV-Visible spectroscopy. Diminution in the value of Do for oxidation indicated the binding of the complex with DNA corresponding to Kb = 8.58 × 104 M-1. UV-Visible spectroscopy yielded ε = 49 L mol-1 cm-1 and Kb = 2.96 × 104 M-1. The data of both techniques support each other. The self-induced redox activation of the complex, as indicated by cyclic voltammetry heralds its potential applications in redox catalysis and anticancer activity.

  13. Near infrared electrochromic naphthalene-based polyimides containing triarylamine: Synthesis and electrochemical properties

    International Nuclear Information System (INIS)

    Cai, Jiwei; Ma, Lina; Niu, Haijun; Zhao, Ping; Lian, Yongfu; Wang, Wen

    2013-01-01

    Graphical abstract: Electrochromic behavior of PI thin film. The inset shows the photographic images of the film at indicated applied voltages. - Highlights: • The polymer films showed reversible electrochemical oxidation, high coloration efficiency (CE), low switching time. • The polyimides revealed multielectrochromic characteristic. • The polyimides were the near-infrared (NIR)-absorbing electrochromic materials. - Abstract: A series of novel multicolored near-infrared (NIR) electrochromic aromatic polyimides (PIs) have been synthesized by a conventional two-step polymerization process. The structures of PIs were characterized by means of Fourier transform infrared (FTIR), 1 H NMR spectroscopy, which showed an agreement with the proposed structure. These poly (amic acid)s have inherent viscosities of 0.75–0.84 dl/g. They are readily soluble in many organic solvents, such as N-methyl-2-pyrrolidone (NMP), dimethylacetamide (DMAc), N,N-dimethylformamide (DMF) and dimethyl sulfoxide (DMSO). All PIs displayed outstanding thermal stabilities, i.e. 5% wt loss in excess of 480 °C under nitrogen. The highest-occupied molecular orbital (HOMO) and lowest-unoccupied molecular orbital (LUMO) energy levels of these PIs were determined in the range of −4.95 to −5.00 and −1.97 to −2.01 eV (vs the vacuum level) by cyclic voltammetry method which were consisting with the results of quantum chemical calculation well, respectively. All obtained PIs revealed stability of electrochromic characteristics, changing color from original yellowish to red and blue. In addition, the PIs films showed high coloration efficiency (CE), short switching time, and anodic electrochromic behavior. The properties prove that the PIs are multipurpose materials which will be subject of hole-transporting and electrochromic application in the near future

  14. Anderson-Type Polyoxometalates Functionalized by Tetrathiafulvalene Groups: Synthesis, Electrochemical Studies, and NLO Properties.

    Science.gov (United States)

    Boulmier, Amandine; Vacher, Antoine; Zang, Dejin; Yang, Shu; Saad, Ali; Marrot, Jérôme; Oms, Olivier; Mialane, Pierre; Ledoux, Isabelle; Ruhlmann, Laurent; Lorcy, Dominique; Dolbecq, Anne

    2018-04-02

    Three polyoxometalates (POMs) functionalized by tetrathiafulvalene (TTF) molecules have been synthesized by a coupling reaction between the Anderson-type POMs [MnMo 6 O 18 {(OCH 2 ) 3 CNH 2 } 2 ] 3- or [AlMo 6 O 18 (OH) 3 {(OCH 2 ) 3 CNH 2 }] 3- and the TTF carboxylic acid derivative (MeS) 3 TTF(S-CH 2 -CO 2 H). The monofunctionalized TTF-AlMo 6 POM contains one TTF group covalently grafted on an Al Anderson platform. The symmetrical TTF-MnMo 6 -TTF POM possesses two TTF groups grafted on each side of a Mn Anderson derivative while the asymmetrical TTF-MnMo 6 -SP POM contains a TTF and a spiropyran groups. These three trianionic species have been characterized by elemental analysis, 1 H and 13 C NMR, FT-IR spectroscopy, ESI-MS spectrometry, and single-crystal X-ray diffraction (for TTF-MnMo 6 -TTF). In the solid state, the grafted TTF molecules of TTF-MnMo 6 -TTF POMs interact via S···S and π···π interactions and form chains. The electrochemical properties of the complexes reflect the contributions of both the inorganic POM and the TTF moieties. Despite adsorption of the oxidized hybrid species on the Pt grid working electrode, UV-vis-NIR spectroelectrochemical investigations evidence peaks characteristic of the oxidation of the TTF units. Finally, hyper-Rayleigh scattering (HRS) measurements show that the three novel TTF derivatives exhibit β values between 20 and 37 × 10 -30 esu. Moreover it is observed that the oxidation of the TTF moieties by Fe 3+ ions increases the NLO response. These values are in the order of magnitude of that found for the well-known 4-dimethylamino- N-methyl-4-stilbazolium (DAS + ) cation (β = 60 × 10 -30 esu).

  15. Synthesis and electrochemical properties of stannous oxide clinopinacoid as anode material for lithium ion batteries.

    Science.gov (United States)

    Iqbal, M Zubair; Wang, Fengping; Rafique, M Yasir; Ali, Shujaat; Din, Rafi Ud; Farooq, M Hassan; Khan, Matiullah; Ali, Murad

    2013-03-01

    Tin monoxide is a significant functional semiconductor material which employed to a wide area of applications especially optical and energy storage devices. Presently, template free hydrothermal technique has been employing to synthesize stannous oxide (SnO) clinopinacoid type controlled morphology using SnCl2 x 2H2O, NH3, and H2O as raw materials. The crystalline phase, morphology, particle size and component were characterized by X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS) and field-emission scanning electron microscopy (FESEM). FESEM results exhibited the large scale homogeneous growth of clinopinacoid architecture with the obvious size of 5 - 7 micrometers. The XRD results showed that the average crystallite size of the tetragonal phase romarchite SnO was about 29 nm calculated from the FWHM of X-ray diffraction pattern. The dominant Raman active modes A(1g) = 205 cm(-1), B(1g) = 105-107 cm(-1) and about 6 cm(-1) redshift were observed by the Raman spectroscopy, which further confirmed the existence of the nano tetragonal phase SnO. The electrochemical performance of as-synthesized SnO clinopinacoid structure as the anode material for lithium ion batteries was investigated. It was observed that the first discharge capacity of the two samples could reach a very high value of 1502 mA h g(-1) and 1422 mA h g(-1) respectively. The effect of nitrogen concentration on morphology as well as cyclic performance of Li-Ion-batteries was also discussed.

  16. Synthesis of tantalum carbide and nitride nanoparticles using a reactive mesoporous template for electrochemical hydrogen evolution

    KAUST Repository

    Alhajri, Nawal Saad

    2013-01-01

    Tantalum carbide and nitride nanocrystals were prepared through the reaction of a tantalum precursor with mesoporous graphitic (mpg)-C 3N4. The effects of the reaction temperature, the ratio of the Ta precursor to the reactive template (mpg-C3N4), and the selection of the carrier gas (Ar, N2 and NH3) on the resultant crystal phases and structures were investigated. The produced samples were characterized using powder X-ray diffraction (XRD), CHN elemental analyses, thermogravimetric analyses (TGA), nitrogen sorption, a temperature-programmed reaction with mass spectroscopy (MS), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM). The results indicate that the different tantalum phases with cubic structure, TaN, Ta2CN, and TaC, can be formed under a flow of nitrogen when formed at different temperatures. The Ta3N5 phase with a Ta5+ oxidation state was solely obtained at 1023 K under a flow of ammonia, which gasified the C 3N4 template and was confirmed by detecting the decomposed gaseous products via MS. Significantly, the formation of TaC, Ta2CN, and TaN can be controlled by altering the weight ratio of the C 3N4 template relative to the Ta precursor at 1573 K under a flow of nitrogen. The high C3N4/Ta precursor ratio generally resulted in high carbide content rather than a nitride one, consistent with the role of mpg-C3N4 as a carbon source. Electrochemical measurements revealed that the synthesized nanomaterials were consistently able to produce hydrogen under acidic conditions (pH 1). The obtained Tafel slope indicates that the rate-determining step is the Volmer discharge step, which is consistent with adsorbed hydrogen being weakly bound to the surface during electrocatalysis. © 2013 The Royal Society of Chemistry.

  17. 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.

  18. Electrochemical synthesis of metallic microstructures using etched ion tracks in nuclear track filters

    International Nuclear Information System (INIS)

    Sanjeev Kumar; Shyam Kumar; Rajesh Kumar; Chakravarti, K.

    2004-01-01

    Interest in nano/microstructures results from their numerous potential applications in various areas such as materials and biomedical sciences, electronics, optics, magnetism, energy storage and electrochemistry. Materials with micro/nanoscopic dimensions not only have potential technological applications in areas such as device technology and drug delivery, but also are of fundamental interest in that the properties of a material can change in this regime of transition between the bulk and molecular scales. Electrodeposition is a versatile technique combining low processing cost with ambient conditions that can be used to prepare metallic, polymeric and semiconducting microstructures. In the present work ion track membranes of Makrofol (KG) have been used as templates for synthesis of metallic microstructures using the technique of electrodeposition. (author)

  19. Sonochemical synthesis of nanostructured nickel hydroxide as an electrode material for improved electrochemical energy storage application

    Directory of Open Access Journals (Sweden)

    Arshid Numan

    2017-08-01

    Full Text Available A facile and fast approach for the synthesis of a nanostructured nickel hydroxide (Ni(OH2 via sonochemical technique is reported in the present study. The X-ray diffraction results confirmed that the synthesized Ni(OH2 was oriented in β-phase of hexagonal brucite structure. The nanostructured Ni(OH2 electrode exhibited the maximum specific capacitance of 1256 F/g at a current density of 200 mA/g in 1 M KOH(aq. Ni(OH2 electrodes exhibited the pseudocapacitive behavior due to the presence of redox reaction. It also exhibited long-term cyclic stability of 85% after 2000 cycles, suggesting that the nanostructured Ni(OH2 electrode will play a promising role for high performance supercapacitor application.

  20. Morphology-Controlled Synthesis of Hematite Nanocrystals and Their Optical, Magnetic and Electrochemical Performance

    Science.gov (United States)

    Li, Bangquan; Sun, Qian; Fan, Hongsheng; Cheng, Ming; Shan, Aixian; Cui, Yimin; Wang, Rongming

    2018-01-01

    A series of α-Fe2O3 nanocrystals (NCs) with fascinating morphologies, such as hollow nanoolives, nanotubes, nanospindles, and nanoplates, were prepared through a simple template-free hydrothermal synthesis process. The results showed that the morphologies could be easily controlled by SO42− and H2PO4−. Physical property analysis showed that the α-Fe2O3 NCs exhibited shape- and size-dependent ferromagnetic and optical behaviors. The absorption band peak of the α-Fe2O3 NCs could be tuned from 320 to 610 nm. Furthermore, when applied as electrode material for supercapacitor, the hollow olive-structure exhibited the highest capacitance (285.9 F·g−1) and an excellent long-term cycling stability (93% after 3000 cycles), indicating that it could serve as a candidate electrode material for a supercapacitor. PMID:29342929

  1. Space-Confined Synthesis of Three-Dimensional Boron/Nitrogen-Doped Carbon Nanotubes/Carbon Nanosheets Line-in-Wall Hybrids and Their Electrochemical Energy Storage Applications

    DEFF Research Database (Denmark)

    Zhu, Shan; Li, Jiajun; Li, Qingfeng

    2016-01-01

    and CNTs in this unique pattern, the LIW-NB integrates advantages of three aspects: first, the doped heteroatoms enhancing electrochemical properties of carbon matrix; second, the warp-proof nanosheets supplying high specific surface area; and the extracted and embedded CNTs serving as electron conductive...... paths and reinforcing the whole architecture. As a result, the 3D LIW-NB shows excellent electrochemical properties: as the electrode of supercapacitors, LIW-NB exhibits high specific capacity at different current densities (389 F g-1 at 1 A g-1 and 129 F g-1 at 20 Ag-1); as the lithium ion battery......This research demonstrates a flexible one-pot strategy for fabricating three-dimensional (3D) boron/nitrogen-doped networks of carbon nanotubes(CNTs)/carbon nanosheets "Line-in-Wall" hybrids (LIWNB) based on the space-confined template method. In the synthesis, the high rate of freezing step...

  2. One-Pot Synthesis of Concave Platinum-Cobalt Nanocrystals and Their Superior Catalytic Performances for Methanol Electrochemical Oxidation and Oxygen Electrochemical Reduction.

    Science.gov (United States)

    Ma, Yanxia; Yin, Lisi; Yang, Tao; Huang, Qingli; He, Maoshuai; Zhao, Hong; Zhang, Dongen; Wang, Mingyan; Tong, Zhiwei

    2017-10-18

    Exploring highly efficient electro-catalysts is of significant urgency for the widespread uptake of the direct methanol fuel cells (DMFCs). Pt-Co nanocrystals have attracted considerable attentions because of their superior catalytic performance toward both methanol oxidation and oxygen reduction in the preliminary assessments. This Research Article presents a Pt-Co bimetal catalyst that is synthesized through a facile coreduction strategy. The Pt-Co nanocrystals have concave cubic shape with a high uniform size of 7-9 nm and Pt-rich surfaces. The catalysis of the concave cubic Pt-Co nanoparticles toward both methanol electrochemical oxidation reaction (MOR) and oxygen electrochemical reduction reaction (ORR) is evaluated. In comparison with the commercial Pt/C catalyst (Johnson Matthey), the present concave cubic Pt-Co catalyst displays superior performances in not only catalytic activity but also durability. The concave Pt-Co catalyst also shows higher activities than spherical and cubic Pt-Co nanoparticles. The dramatic enhancement is mainly attributed to its alloyed composition, Pt-rich surface and the concave nanostructure. The results of our research indicate that the concave Pt-Co nanocrystal could be a promising catalyst for both MOR and ORR. The present work might also raise more concerns on exploiting morphology and composition of nanocrystal catalysts, which are expected to provide high catalytic performance in electrochemical reactions.

  3. Synthesis and characterization of electrochemically deposited nanocrystalline CdTe thin films

    International Nuclear Information System (INIS)

    Singh, Ragini Raj; Painuly, Diksha; Pandey, R.K.

    2009-01-01

    Electrodeposition is emerging as a method for the synthesis of semiconductor thin films and nanostructures. In this work we prepared the nanocrystalline CdTe thin films on indium tin oxide coated glass substrate from aqueous acidic bath at the deposition temperature 50 ± 1 deg. C. The films were grown potentiostatically from -0.60 V to -0.82 V with respect to saturated calomel reference electrode. The structural, compositional, morphological and optical properties were investigated using X-ray diffraction (XRD), energy dispersive analysis by X-rays (EDAX), atomic force microscopy (AFM), and UV-vis spectroscopy respectively and cyclic voltammetery. The structural and optical studies revealed that films are nanocrystalline in nature and possess cubic phase, also the films are preferentially oriented along the cubic (1 1 1) plane. The effect of cadmium composition on the deposited morphology was also investigated. The size dependent blue shift in the experimentally determined absorption edge has been compared with the theoretical predictions based on the effective mass approximation and tight binding approximation. It is shown that the experimentally determined absorption edges depart from the theoretically calculated values.

  4. Electrochemical synthesis and characterization of zinc carbonate and zinc oxide nanoparticles

    Science.gov (United States)

    Pourmortazavi, Seied Mahdi; Marashianpour, Zahra; Karimi, Meisam Sadeghpour; Mohammad-Zadeh, Mohammad

    2015-11-01

    Zinc oxide and its precursor i.e., zinc carbonate is widely utilized in various fields of industry, especially in solar energy conversion, optical, and inorganic pigments. In this work, a facile and clean electrodeposition method was utilized for the synthesis of zinc carbonate nanoparticles. Also, zinc oxide nanoparticles were produced by calcination of the prepared zinc carbonate powder. Zinc carbonate nanoparticles with different sizes were electrodeposited by electrolysis of a zinc plate as anode in the solution of sodium carbonate. It was found that the particle size of zinc carbonate might be tuned by process parameters, i.e., electrolysis voltage, carbonate ion concentration, solvent composition and stirring rate of the electrolyte solution. An orthogonal array design was utilized to identify the optimum experimental conditions. The experimental results showed that the minimum size of the electrodeposited ZnCO3 particles is about 24 nm whereas the maximum particle size is around 40 nm. The TG-DSC studies of the nanoparticles indicated that the main thermal degradation of ZnCO3 occurs in two steps over the temperature ranges of 150-250 and 350-400 °C. The electrosynthesized ZnCO3 nanoparticles were calcined at the temperature of 600 °C to prepare ZnO nanoparticles. The prepared ZnCO3 and ZnO nanoparticles were characterized by SEM, X-ray diffraction (XRD), and FT-IR techniques.

  5. Synthesis, electrochemical and photophysical properties of heterodinuclear Ru-Mn and Ru-Zn complexes bearing ambident Schiff base ligand.

    Science.gov (United States)

    Guillo, Pascal; Hamelin, Olivier; Loiseau, Frédérique; Pécaut, Jacques; Ménage, Stéphane

    2010-06-28

    While ruthenium tris(diimine) complexes have been extensively studied, this is not the case with ruthenium bis(diimine)X(2) complexes where X represents a pyridinyl-based ligand. The synthesis of a new complex ([2][PF(6)](2)) bearing two ambident Schiff base ligands (HL) constituted by the assembly of phenol and pyridinyl moieties is reported. Thanks to the heteroditopic property of HL, compound [2](2+) was used as an original metalloligand for the coordination of a redox-active (Mn(III)) and redox-inactive (Zn(II)) second metal cation affording three heterodinuclear complexes, namely, [(bpy)(2)Ru(2)Mn(acac)][PF(6)](2) ([3][PF(6)](2); acac = acetylacetonate), [(bpy)(2)Ru(2)Mn(OAc)][PF(6)](2) ([4][PF(6)](2), OAc = acetate), and [(bpy)(2)Ru(2)Zn][PF(6)](2) ([5][PF(6)](2)). The influence of the second metal with regard to the photophysical and electrochemical properties of the ruthenium bis(diimine)X(2) subunit was then investigated. In the case of Ru(II)-Mn(III) heterodinuclear complexes, a partial quenching of the luminescence was observed as a consequence of an efficient electron transfer process from the ruthenium to the manganese. EPR and spectrophotometric analyses of the oxidized species resulting from the one-electron oxidation of compounds [3](2+) and [4](2+) showed the formation of a Mn(IV) species for [3](2+) and an organic free radical for [4](2+).

  6. 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

  7. 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

  8. Synthesis of CdS flower-like hierarchical microspheres as electrode material for electrochemical performance

    Energy Technology Data Exchange (ETDEWEB)

    Kaviyarasu, K., E-mail: Kaviyarasuloyolacollege@gmail.com [UNESCO-UNISA Africa Chair in Nanosciences/Nanotechnology Laboratories, College of Graduate Studies, University of South Africa (UNISA), Muckleneuk Ridge, P O Box 392, Pretoria (South Africa); Nanosciences African Network (NANOAFNET), Materials Research Department (MSD), iThemba LABS-National Research Foundation - NRF, 1 Old Faure Road, 7129, P O Box 722, Somerset West, Western Cape Province (South Africa); Manikandan, E., E-mail: maniphysics@gmail.com [Nanosciences African Network (NANOAFNET), Materials Research Department (MSD), iThemba LABS-National Research Foundation - NRF, 1 Old Faure Road, 7129, P O Box 722, Somerset West, Western Cape Province (South Africa); Central Research Laboratory, Sree Balaji Medical College & Hospital, Bharath University, Chrompet, Chennai, 600044, Tamil Nadu (India); Maaza, M., E-mail: maaza@gmail.com [UNESCO-UNISA Africa Chair in Nanosciences/Nanotechnology Laboratories, College of Graduate Studies, University of South Africa (UNISA), Muckleneuk Ridge, P O Box 392, Pretoria (South Africa); Nanosciences African Network (NANOAFNET), Materials Research Department (MSD), iThemba LABS-National Research Foundation - NRF, 1 Old Faure Road, 7129, P O Box 722, Somerset West, Western Cape Province (South Africa)

    2015-11-05

    We report in this paper, a facile hydrothermal route for the preparation of CdS nanocrystals at room temperature (RT). Composition, structure and morphology of the products were analyzed and characterized by X-ray diffraction (XRD) confirms that the hydrothermal treatment at 180 °C for periods ranging from 0 to 1440 min caused no significant modification of the long range order structure subjected to hydrothermal treatment. From the XRD analysis the diffraction peaks pertaining to 26.75°, 43.89° and 52.34° are attributed to the (111), (220) and (311) planes of cubic zinc blende structure. The Photoluminescence (PL) spectra are dominated by a strong narrow band edge emission tunable in the blue region of the visible spectra indicating the narrow size distribution of CdS nanocrystals. TEM observation shows that the CdS nanocrystals synthesized by hydrothermal synthesis are well dispersed and the average crystallite size was found to be ∼10 nm. The confocal microscopic studies reveal that each flower like spheres is due to Ostwald's ripening with numerous nanoparticles aggregating a surface. - Highlights: • The adjacent particle coalesces together forming spherical particles. • The average crystalline size of CdS nanoparticles was found to be ∼3 nm. • In the case of spherical crystallite, is given by L = 3/4 D. • The CdS nanocrystal exhibits a direct band gap of 2.4 eV. • The microspheres are dispersed with good monodispersity.

  9. 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

  10. Radiation Synthesis of Selective Ion exchange Membranes for Different Electrochemical Applications

    International Nuclear Information System (INIS)

    Khozemy, E.E.Z.

    2013-01-01

    The polymer electrolyte membranes (PEMs) has gain considerable attention due to its applications in many energy related fields such as water electorlyzers, fuel cells, battery systems, etc. Polymer electrolyte membranes exhibit several advantages over liquid or solid inorganic electrolytes such as high proton conductivity, good chemical, thermal and mechanical properties, because this technique allows us to introduce ion conducting (electrolytes) regions directly into polymer films which have excellent thermal and mechanical properties. An ion-exchange membrane is the key component in polymer electrolyte membranes and can be used in a number in different processes. However, in all these processes membrane carrying electrical charges are used to control the transport of ionic species and separate them selectively. Ion-exchange membrane separation processes can be classified according to their application into three categories: 1- Mass separation processes such as electrodialysis 2- Chemical synthesis process such as the chlorine alkaline electrolysis 3- Energy conversion and storage process such as fuel cells and electrical batteries. Commercial PEMs are based mainly on perfluorinated membrane materials, such as Nafion. Disadvantages of these perfluorinated membrane materials are: expensive due to the complex fluorine chemistry, also methanol crossover. These factors, in addition to environmental recycling difficulties of perfluorinated membranes, have combined to limit their widespread commercial application in PEMFC. The main disadvantage associated with PTFE is that it exclusively undergoes main-chain scission due to the relatively stronger C–F bond as compared with the C–C bond, and a relatively low irradiation dose can effectively reduce the molecular weight of the PTFE. Thus, the present work is aiming to prepare inexpensive and good thermal and mechanical polymer electrolyte membranes. Radiation induced grafting of styrene onto polyethylene (PE

  11. 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.

  12. 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

  13. 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.

  14. 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.

  15. Hydrothermal synthesis of α-Ni(OH){sub 2} and its conversion to NiO with electrochemical properties

    Energy Technology Data Exchange (ETDEWEB)

    Cai, Yong; Ma, Jianmin, E-mail: nanoelechem@hnu.edu.cn; Wang, Taihong, E-mail: thwang@hnu.edu.cn

    2014-01-05

    Highlights: • α-Ni(OH){sub 2} microspheres have been synthesized with triethanolamine. • The formation mechanism of α-Ni(OH){sub 2} microspheres is suggested. • NiO deriving from α-Ni(OH){sub 2} microspheres exhibits better electrochemical performances. -- Abstract: The paper reports the fabrication of microscale NiO matrixes with enhanced electrochemical properties through annealing the corresponding chrysanthemum-like α-Ni(OH){sub 2} microspheres. The precursor α-Ni(OH){sub 2} can be synthesized by a hydrothermal method using triethanolamine as the alkaline source. The formation mechanism of chrysanthemum-like α-Ni(OH){sub 2} microspheres is properly discussed. Furthermore, the electrochemical experiments demonstrate that the microscale NiO matrixes show superior electrochemical behavior in lithium-ion batteries due to their unique structures.

  16. 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.

  17. 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

  18. High loading MnO2 nanowires on graphene paper: facile electrochemical synthesis and use as flexible electrode for tracking hydrogen peroxide secretion in live cells.

    Science.gov (United States)

    Dong, Shuang; Xi, Jiangbo; Wu, Yanan; Liu, Hongwei; Fu, Chaoyang; Liu, Hongfang; Xiao, Fei

    2015-01-01

    Recent progress in flexible and lightweight electrochemical sensor systems requires the development of paper-like electrode materials. Here, we report a facile and green synthesis of a new type of MnO2 nanowires-graphene nanohybrid paper by one-step electrochemical method. This strategy demonstrates a collection of unique features including the effective electrochemical reduction of graphene oxide (GO) paper and the high loading of MnO2 nanowires on electrochemical reduced GO (ERGO) paper. When used as flexible electrode for nonenzymatic detection of hydrogen peroxide (H2O2), MnO2-ERGO paper exhibits high electrocatalytic activity toward the redox of H2O2 as well as excellent stability, selectivity and reproducibility. The amperometric responses are linearly proportional to H2O2 concentration in the range 0.1-45.4 mM, with a detection limit of 10 μM (S/N=3) and detection sensitivity of 59.0 μA cm(-2) mM(-1). These outstanding sensing performances enable the practical application of MnO2-ERGO paper electrode for the real-time tracking H2O2 secretion by live cells macrophages. Therefore, the proposed graphene-based nanohybrid paper electrode with intrinsic flexibility, tailorable shapes and adjustable properties can contribute to the full realization of high-performance flexible electrode material used in point-of-care testing devices and portable instruments for in-vivo clinical diagnostics and on-site environmental monitoring. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. 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.

  20. Synthesis of free-standing metal sulfide nanoarrays via anion exchange reaction and their electrochemical energy storage application.

    Science.gov (United States)

    Xia, Xinhui; Zhu, Changrong; Luo, Jingshan; Zeng, Zhiyuan; Guan, Cao; Ng, Chin Fan; Zhang, Hua; Fan, Hong Jin

    2014-02-26

    Metal sulfides are an emerging class of high-performance electrode materials for solar cells and electrochemical energy storage devices. Here, a facile and powerful method based on anion exchange reactions is reported to achieve metal sulfide nanoarrays through a topotactical transformation from their metal oxide and hydroxide preforms. Demonstrations are made to CoS and NiS nanowires, nanowalls, and core-branch nanotrees on carbon cloth and nickel foam substrates. The sulfide nanoarrays exhibit superior redox reactivity for electrochemical energy storage. The self-supported CoS nanowire arrays are tested as the pseudo-capacitor cathode, which demonstrate enhanced high-rate specific capacities and better cycle life as compared to the powder counterparts. The outstanding electrochemical properties of the sulfide nanoarrays are a consequence of the preservation of the nanoarray architecture and rigid connection with the current collector after the anion exchange reactions.

  1. 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.

  2. 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

  3. 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)

  4. 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.

  5. Highly Ordered Vertical Arrays of TiO2/ZnO Hybrid Nanowires: Synthesis and Electrochemical Characterization.

    Science.gov (United States)

    Gujarati, Tanvi P; Ashish, Ajithan G; Rai, Maniratnam; Shaijumon, Manikoth M

    2015-08-01

    We report the fabrication of vertically aligned hierarchical arrays of TiO2/ZnO hybrid nanowires, consisting of ZnO nanowires grown directly from within the pores of TiO2 nanotubes, through a combination of electrochemical anodization and hydrothermal techniques. These novel nano-architectured hybrid nanowires with its unique properties show promise as high performance supercapacitor electrodes. The electrochemical behaviour of these hybrid nanowires has been studied using Cyclic voltammetry, Galvanostatic charge-discharge and Electrochemical impedance spectroscopy (EIS) measurements using 1.5 M tetraethylammoniumtetrafluoroborate in acetonitrile as the electrolyte. Excellent electrochemical performances with a maximum specific capacitance of 2.6 mF cm-2 at a current density of 10 µA cm-2, along with exceptional cyclic stability, have been obtained for TiO2/ZnO-1 h hybrid material. The obtained results demonstrate the possibility of fabricating new geometrical architectures of inorganic hybrid nanowires with well adhered interfaces for the development of hybrid energy devices.

  6. 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.

  7. 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.

  8. 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.

  9. Synthesis and electrochemical properties of LiMn2O4 and LiCoO2-coated LiMn2O4 cathode materials

    International Nuclear Information System (INIS)

    Wang Hongen; Qian Dong; Lu Zhouguang; Li Yongkun

    2012-01-01

    Highlights: ► Spinel LiMn 2 O 4 with different morphologies have been synthesized. ► LiCoO 2 -coated LiMn 2 O 4 was prepared by a sol–gel route. ► LiMn 2 O 4 and LiCoO 2 -coated LiMn 2 O 4 microspheres display much better electrochemical cycling properties than those of LiMn 2 O 4 octahedrons. - Abstract: The synthesis of spinel LiMn 2 O 4 material by a spherical MnO 2 precursor route is reported in this paper. Hydrothermal and solid-state reactions were adopted to investigate the effects of synthetic methods on the morphologies and electrochemical characteristics of the LiMn 2 O 4 products, respectively. LiCoO 2 -coated LiMn 2 O 4 microspheres were also prepared by a sol–gel route based on the as-prepared LiMn 2 O 4 microspheres. The products were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectrum (EDX), and inductively-coupled plasma emission spectrograph (ICP-ES). The results show that LiMn 2 O 4 octahedrons can be obtained under hydrothermal conditions while LiMn 2 O 4 microspheres can be prepared by the solid-state reaction. Electrochemical characterization reveals that the resulting LiMn 2 O 4 microspheres and LiCoO 2 -coated LiMn 2 O 4 microspheres display much better cycling properties than those of LiMn 2 O 4 octahedrons.

  10. ELECTROCHEMICAL PROPERTIES AND ELECTROCHEMICAL ...

    African Journals Online (AJOL)

    Rct is about five times higher in acetonitrile relative to water. All these EIS results of the different types of PPy suggest a relation with the wettability of the polymer. KEY WORDS: Conducting polymers, Polypyrrole, Electrochemical impedance spectroscopy, Equivalent- electrical circuit, Micellar media. INTRODUCTION.

  11. Synthesis and electrochemical properties of Na1.2V3O8/LTX as anodic material in sodium ion batteries

    Directory of Open Access Journals (Sweden)

    Stojković-Simatović Ivana B.

    2016-01-01

    Full Text Available In this paper, the synthesis of composite Na1.2V3O8/LTX by sol-gel method was described. The synthesized powders were characterized by X-ray powder diffraction (XRD and thermogravimetric analysis (TGA while the electrochemical performances were investigated by cycling voltammetry (CV by different scan rate. After thermal treatment, the part of carbon was 7%. The initial discharge capacity was 100.44 mAhg-1. The most capacity fade was after 2nd cycle (14% but capacity fade from 6th to 10th cycle was only 10%. The efficiency of Na1.2V3O8/LTX is around 95%.

  12. 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.

  13. Synthesis of highly stable sub-8 nm TiO2 nanoparticles and their multilayer electrodes of TiO2/MWNT for electrochemical applications.

    Science.gov (United States)

    Hyder, Md Nasim; Gallant, Betar M; Shah, Nisarg J; Shao-Horn, Yang; Hammond, Paula T

    2013-10-09

    Next-generation electrochemical energy storage for integrated microsystems and consumer electronic devices requires novel electrode materials with engineered architectures to meet the requirements of high performance, low cost, and robustness. However, conventional electrode fabrication processes such as doctor blading afford limited control over the electrode thickness and structure at the nanoscale and require the incorporation of insulating binder and other additives, which can promote agglomeration and reduce active surface area, limiting the inherent advantages attainable from nanoscale materials. We have engineered a route for the synthesis of highly stable, sub-8 nm TiO2 nanoparticles and their subsequent incorporation with acid-functionalized multiwalled carbon nanotubes (MWNTs) into nanostructured electrodes using aqueous-based layer-by-layer electrostatic self-assembly. Using this approach, binder-free thin film electrodes with highly controllable thicknesses up to the micrometer scale were developed with well-dispersed, nonagglomerated TiO2 nanoparticles on MWNTs. Upon testing in an Li electrochemical half-cell, these electrodes demonstrate high capacity (>150 mAh/gel(ectrode) at 0.1 A/gel(ectrode)), good rate capability (>100 mAh/gel(ectrode) up to 1 A/g(electrode)) and nearly no capacity loss up to 200 cycles for electrodes with thicknesses up to 1480 nm, indicating their promise as thin-film negative electrodes for future Li storage applications.

  14. Facile Synthesis of Three-Dimensional Sandwiched MnO2@GCs@MnO2Hybrid Nanostructured Electrode for Electrochemical Capacitors.

    Science.gov (United States)

    Jian, Xian; Liu, Shiyu; Gao, Yuqi; Zhang, Wanli; He, Weidong; Mahmood, Asif; M Subramaniyam, Chandrasekar; Wang, Xiaolin; Mahmood, Nasir; Dou, Shi Xue

    2017-06-07

    Designable control over the morphology and structure of active materials is highly desirable for achieving high-performance devices. Here, we develop a facile microwave-assisted synthesis to decorate MnO 2 nanocrystals on three-dimensional (3D) graphite-like capsules (GCs) to obtain sandwich nanostructures (3D MnO 2 @GCs@MnO 2 ) as electrode materials for electrochemical capacitors (ECs). A templated growth of the 3D GCs was carried out via catalytic chemical vapor deposition and MnO 2 was decorated on the exterior and interior surfaces of the GC walls through microwave irradiation to build an engineered architecture with robust structural and morphological stability. The unique sandwiched architecture has a large interfacial surface area, and allows for rapid electrolyte diffusion through its hollow/open framework and fast electronic motion via the carbon backbone. Furthermore, the tough and rigid nature of GCs provides the necessary structural stability, and the strong synergy between MnO 2 and GCs leads to high electrochemical activity in both neutral (265.1 F/g at 0.5 A/g) and alkaline (390 F/g at 0.5 A/g) electrolytes. The developed hybrid exhibits stable capacitance up to 6000 cycles in 1 M Na 2 SO 4 . The hybrid is a potential candidate for future ECs and the present study opens up an effective avenue to design hybrid materials for various applications.

  15. 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.

  16. 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.

  17. 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.

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

    Science.gov (United States)

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

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

  19. 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

  20. 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.

  1. Electrochemical hydrogen storage properties of Mg100−xNix produced by hydriding combustion synthesis and mechanical milling

    Directory of Open Access Journals (Sweden)

    Delong Zhu

    2017-02-01

    Full Text Available In this work, Mg-based hydrogen storage composites with an initial 100-x: x (x=25, 32.3, 50, 66.7 of Mg:Ni molar ratio were prepared by HCS+MM and their phase compositions and electrochemical performances were investigated in detail. The results show that the composites with desirable constituents can be achieved by adjusting the molar ratio of the starting materials in the HCS process. Particularly, the HCS product of Mg67.7Ni32.3 consists of the principal phase Mg2NiH4 and minor phase Mg2NiH0.3. The dominate phase varies from Mg2NiH0.3 and MgH2 for the Mg enriched sample (x32.3. The MM modification not only brings about grain refinement of the alloys, but also leads to phase transformation of part Mg2NiH4 to Mg2NiH0.3 in the Mg67.7Ni32.3 sample. Electrochemical tests indicate that each sample can reach its maximum discharge capacity at the first cycle. Mg67.7Ni32.3 displays the highest discharge capacity as well as a superior electrochemical kinetics owing to its excellent H atom diffusion ability and lower charge-transfer resistance. The Mg67.7Ni32.3 provides the most optimized Mg/Ni atomic ratio considering the comprehensive electrochemical properties of all samples.

  2. Electrochemical Synthesis of N-Methylpyrrole and N-Methylcarbazole Copolymer on Carbon Fiber Microelectrodes, and Their Characterization

    OpenAIRE

    SARAÇ, A. Sezai; DOĞRU, Erkan; ATEŞ, Murat; PARLAK, Elif ALTÜRK

    2014-01-01

    Copolymer films of N-methylpyrrole (N-MPy) and N-methylcarbazole (N-MCz) were synthesized electrochemically onto single carbon fiber microelectrodes (CFMEs). Deposition conditions on the carbon fiber, influence of the monomer concentrations on the copolymerization of P[N-methylpyrrole-co-N-methylcarbazole] P[N-MPy-co-N-MCz], and the electrochemistry of the resulting homopolymer and copolymers were studied using cyclic voltammetry, FTIR-ATR, in-situ spectroelectrochemistry, a UV-vis sp...

  3. Synthesis and electrochemical characterization of nanosized Li2MnO3 cathode material for lithium ion batteries

    Science.gov (United States)

    Li, Shiyou; Lei, Dan

    2017-10-01

    A simple one-step solid state reaction way of preparing Nano sized Li2MnO3 powders is investigated. Synthesized products were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). In addition, we have observed that the inferior electrochemical performance of Li2MnO3 upon cycling was attributed to the structural degradation caused by migration of the transition metal (Mn) into the Li layer and repetitive shearing of oxygen layers.

  4. 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.

  5. 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.%.

  6. Synthesis of novel ZnV₂O₄ hierarchical nanospheres and their applications as electrochemical supercapacitor and hydrogen storage material.

    Science.gov (United States)

    Butt, Faheem K; Tahir, Muhammad; Cao, Chuanbao; Idrees, Faryal; Ahmed, R; Khan, Waheed S; Ali, Zulfiqar; Mahmood, Nasir; Tanveer, M; Mahmood, Asif; Aslam, Imran

    2014-08-27

    Hierarchical nanostructures (Hs) have recently garnered enormous attention due to their remarkable performances in catalysis, electronic devices, energy storage and conversion. Considering the advantage of hierarchical nanostructures, we have formulated a facile and template free method to synthesize novel hierarchical nanospheres (NHNs) of ZnV2O4. Both zinc and vanadium are earth abundant, relatively economical and can offer several oxidation states, which can render a broad range of redox reactions favorable for electrochemical energy storage applications. Keeping these points in mind, we investigated for the first time the electrochemical supercapacitor performance of NHNs. The electrochemical measurements were performed in 2 M KOH solution. The measured specific capacitance of ZnV2O4 electrode is 360 F/g at 1 A/g with good stability and retention capacity of 89% after 1000 cycles. Moreover, the hydrogen storage properties of NHNs were measured at 473, 573, and 623 K with an absorption of 1.76, 2.03, and 2.49 wt %. respectively. These studies pave the way to consider ZnV2O4 as prospective material for energy storage applications.

  7. 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

  8. Electrochemical synthesis and characterization of poly(3,4-ethylenedioxythiophene) doped with sulfonated calixarenes and sulfonated calixarene–fullerene complexes

    International Nuclear Information System (INIS)

    Dumitriu, Cristina; Mousavi, Zekra; Latonen, Rose-Marie; Bobacka, Johan; Demetrescu, Ioana

    2013-01-01

    Highlights: • PEDOT–C 60 composites were electrosynthesized from aqueous solution. • The surface morphology of PEDOT doped with sulfonated calixarene–C 60 complexes is very similar to that of PEDOT doped with the same sulfonated calixarenes without C 60 . • A remarkable increase in the electroactivity of PEDOT after contact with C 60 in organic solution was observed, which is interesting both from a fundamental point of view and for charge storage applications. -- Abstract: Poly(3,4-ethylenedioxythiophene) (PEDOT) films were electrochemically deposited on glassy carbon (GC) disk electrodes using aqueous solutions containing 3,4-ethylenedioxythiophene (EDOT) and sulfonated calixarenes or fullerene-sulfonated calixarene (C 60 –calixarene) complexes. The EDOT monomer was added to aqueous sulfonated calixarene solutions with and without C 60 and from these solutions PEDOT(calixarene) and PEDOT(C 60 –calixarene) films were electrochemically deposited on GC disk electrodes. The electrochemical properties of GC/PEDOT(C 60 –calixarene) were compared with those of GC/PEDOT doped with other ions, both in aqueous and organic electrolyte solutions using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). CV measurements carried out on GC/PEDOT(C 60 –calixarene) in 0.1 M aqueous KCl solution showed a reduction peak at ca. −0.55 V vs. Ag/AgCl/3 M KCl only during the first potential scan. This was attributed to the irreversible reduction of C 60 to C 60 − inside the PEDOT film. This additional reduction peak was, however, not observed when recording the CVs in organic solution, indicating that C 60 was dissolved from the PEDOT film into the organic electrolyte solution, that is a good solvent for C 60 . When performing CV measurements in an organic electrolyte solution containing C 60 , all GC/PEDOT electrodes with various doping ions and bare GC electrodes showed a reversible reduction peak characteristic for the C 60 /C 60 − redox

  9. Freeze drying synthesis of Li3MnO4 cathode material for Li-ion batteries: A physico-electrochemical study

    International Nuclear Information System (INIS)

    Surace, Yuri; Simões, Mário; Karvonen, Lassi; Yoon, Songhak; Pokrant, Simone; Weidenkaff, Anke

    2015-01-01

    Highlights: • Facilitated synthesis of Li 3 MnO 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 3 MnO 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 −1 ). Li 3 MnO 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 −1 and up to 31% at 50 A kg −1 with a maximum discharge capacity of 290 A h kg −1 ) and the rate capability

  10. 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.

  11. 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.

  12. 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.

  13. Synthesis of Bilayer Graphene on 90/10 Copper (Cu)/Nickel (Ni) Alloy and Transfer by Electrochemical Delamination

    Science.gov (United States)

    2017-09-01

    Road Adelphi, MD 20783-1138 8. PERFORMING ORGANIZATION REPORT NUMBER ARL-TR-8144 9. SPONSORING/MONITORING AGENCY NAME(S) AND ADDRESS(ES) 10... Coating 2 2.3 Transfer Methods 3 2.3.1 Conventional Etch 3 2.3.2 Electrochemical 3 2.4 Characterization 4 3. Results 4 3.1 PMMA Coating 4 3.2...composition were prepared in-house by sputter coating Cu and Ni on a thermally oxidized silicon (Si) substrate (280-nm SiO2) using an AJA

  14. 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.

  15. Electrochemical properties and electrochemical impedance ...

    African Journals Online (AJOL)

    Polypyrrole (PPy) films of different thickness were characterized by electrochemical impedance spectroscopy (EIS) measurements in acetonitrile and aqueous solutions, containing 0.1 M NaClO4 or sodium dodecylsulfate as the dopant. The PPy films were electrochemically deposited on Pt, and their electrochemical ...

  16. Efficient solar-driven synthesis, carbon capture, and desalinization, STEP: solar thermal electrochemical production of fuels, metals, bleach.

    Science.gov (United States)

    Licht, S

    2011-12-15

    STEP (solar thermal electrochemical production) theory is derived and experimentally verified for the electrosynthesis of energetic molecules at solar energy efficiency greater than any photovoltaic conversion efficiency. In STEP the efficient formation of metals, fuels, chlorine, and carbon capture is driven by solar thermal heated endothermic electrolyses of concentrated reactants occuring at a voltage below that of the room temperature energy stored in the products. One example is CO(2) , which is reduced to either fuels or storable carbon at a solar efficiency of over 50% due to a synergy of efficient solar thermal absorption and electrochemical conversion at high temperature and reactant concentration. CO(2) -free production of iron by STEP, from iron ore, occurs via Fe(III) in molten carbonate. Water is efficiently split to hydrogen by molten hydroxide electrolysis, and chlorine, sodium, and magnesium from molten chlorides. A pathway is provided for the STEP decrease of atmospheric carbon dioxide levels to pre-industial age levels in 10 years. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Science.gov (United States)

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

    2017-05-01

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

  18. A High Molar Extinction Coefficient Mono-Anthracenyl Bipyridyl Heteroleptic Ruthenium(II Complex: Synthesis, Photophysical and Electrochemical Properties

    Directory of Open Access Journals (Sweden)

    Peter A. Ajibade

    2011-06-01

    Full Text Available In our quest to develop good materials as photosensitizers for photovoltaic dye-sensitized solar cells (DSSCs, cis-dithiocyanato-4-(2,3-dimethylacrylic acid-2,2'-bipyridyl-4-(9-anthracenyl-(2,3-dimethylacrylic-2,2'-bipyridyl ruthenium(II complex, a high molar extinction coefficient charge transfer sensitizer, was designed, synthesized and characterized by spectroscopy and electrochemical techniques. Earlier studies on heteroleptic ruthenium(II complex analogues containing functionalized oligo-anthracenyl phenanthroline ligands have been reported and documented. Based on a general linear correlation between increase in the length of π-conjugation bond and the molar extinction coefficients, herein, we report the photophysical and electrochemical properties of a Ru(II bipyridyl complex analogue with a single functionalized anthracenyl unit. Interestingly, the complex shows better broad and intense metal-to ligand charge transfer (MLCT band absorption with higher molar extinction coefficient (λmax = 518 nm, e = 44900 M−1cm−1, and appreciable photoluminescence spanning the visible region than those containing higher anthracenyl units. It was shown that molar absorption coefficient of the complexes may not be solely depended on the extended π-conjugation but are reduced by molecular aggregation in the molecules.

  19. 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.

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

    Science.gov (United States)

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

    2017-11-01

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

  1. In-situ hydrothermal synthesis of three-dimensional MnO2-CNT nanocomposites and their electrochemical properties

    International Nuclear Information System (INIS)

    Teng, Fei; Santhanagopalan, Sunand; Wang, Ying; Meng, Dennis Desheng

    2010-01-01

    Three-dimensional (3-D) MnO 2 -carbon nanotube (CNT) nanocomposites were prepared by a simple one-pot hydrothermal method. An electrode was then prepared with these nanocomposites. For comparative investigation, MnO 2 microspheres were also hydrothermally prepared without adding CNTs. The as-synthesized MnO 2 microspheres were then mechanically mixed with CNTs to prepare a subsequent electrode. The samples were characterized by electron microscopy, X-ray diffraction, and electrochemical methods. It has been revealed that a 3-D conductive network of CNTs was formed with microspheres of MnO 2 nanorods interwoven with and connected by CNTs. As a result, the hydrothermally mixed MnO 2 -CNT electrode showed a higher specific capacitance than the mechanically mixed electrode. It has therefore been concluded that the hydrothermal mixing method yields a more homogeneous product that is better suited to take full advantages of both the high capacitance of MnO 2 and the high electrical conductivity of CNTs. The 3-D MnO 2 -CNT nanocomposites reported herein have provided a promising electrode material for supercapacitors and other electrochemical energy storage/conversion devices.

  2. Solvothermal synthesis, electromagnetic and electrochemical properties of jellylike cylinder graphene-Mn3O4 composite with highly coupled effect

    Science.gov (United States)

    Long, Yuting; Xie, Junliang; Li, Hong; Liu, Zirui; Xie, Yahong

    2017-12-01

    Jellylike cylinder graphene-Mn3O4 composite with highly coupled effect was successfully synthesized by a simple solvothermal process. Without using toxic reducing agent and expensive equipment, this method is environmental compatible and suitable for low cost mass production. High capacitance Mn3O4 nanoparticles are homogeneously anchored on excellent conductivity graphene framework and a growth mechanism is hypothesized. Excellent electron conductivity and unique structure of Mn3O4-graphene composite give rise to various applications such as microwave absorber and electrode material. As a microwave absorber, the composite exhibits lowest reflection loss of -14.2 dB in the frequency range of 2-18 GHz. Good microwave absorption performance is due to the structure of the composite where conductive channels form between nano sized Mn3O4 and high conductivity graphene with defects and dangling bonds. As for electrochemical property, Mn3O4-graphene composite with coupled effect shows excellent performance with highest specific capacitance of 246.7 F g-1 in saturated K2SO4 at a scan rate of 5 mV s-1. Good electrochemical property is also attributed to the structure with high utilization of Mn3O4, fast charge carrier transmission, and excellent electronic conductivity. This composite shows a promising application in absorbing materials and electrodes.

  3. Synthesis and characterization of NiCo2O4 nanoplates as efficient electrode materials for electrochemical supercapacitors

    International Nuclear Information System (INIS)

    Kim, Taehyun; Ramadoss, Ananthakumar; Saravanakumar, Balasubramaniam; Veerasubramani, Ganesh Kumar; Kim, Sang Jae

    2016-01-01

    Highlights: • NiCo 2 O 4 nanoplates were synthesized through a facile approach. • The NiCo 2 O 4 nanoplates electrode material exhibit a specific capacitance of 332 F g −1 at 5 mV s −1 . • The fabricated NiCo 2 O 4 electrode reveals 86% retention of initial capacitance after 2000 cycles. - Abstract: In the present work, NiCo 2 O 4 nanoplates were prepared by a facile, low temperature, hydrothermal method, followed by thermal annealing and used supercapacitor applications. The physico-chemical characterization of as-prepared materials were investigated by means of X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FT-IR) and field emission scanning electron microscopy (FE-SEM). The electrochemical measurements demonstrate that the NiCo 2 O 4 nanoplates electrode (NC-5) exhibits a high specific capacitance of 332 F g −1 at a scan rate of 5 mV s −1 and also retained about 86% of the initial specific capacitance value even after 2000 cycles at a current density of 2.5 A g −1 . These results suggest that the fabricated electrode material has huge potential as a novel electrode material for electrochemical capacitors.

  4. Electrochemical Synthesis of Core-Shell-Structured NbC-Fe Composite Powder for Enforcement in Low-Carbon Steel.

    Science.gov (United States)

    Li, Hongmei; Song, Qiushi; Xu, Qian; Chen, Ying; Xu, Liang; Man, Tiannan

    2017-11-01

    An NbC-Fe composite powder was synthesized from an Nb₂O₅/Fe/C mixture by electrochemical reduction and subsequent carbonization in molten CaCl₂-NaCl. The composite has a core-shell structure, in which NbC acts as the cores distributing in the Fe matrix. A strong bonding between NbC and Fe is benefit from the core-shell structure. The sintering and electrochemical reduction processes were investigated to probe the mechanism for the reactions. The results show that NbC particles about several nanometers were embraced by the Fe shell to form a composite about 100 nm in size. This featured structure can feasibly improve the wettability and sinterability of NbC as well as the uniform distribution of the carbide in the cast steel. By adding the composite into steel in the casting process, the grain size of the casted steel was markedly deceased from 1 mm to 500 μm on average, favoring the hardening of the casted steel.

  5. 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.

  6. KH2PO4-Assisted Synthesis and Electrochemical Performance of Highly Uniform CuBi2O4 Microspheres Hierarchically Self-Assembled by Nanoparticles

    Science.gov (United States)

    Wang, Fei; Yang, Hua; Zhang, Yunchuan; Zhang, Haimin

    2017-08-01

    The effect of KH2PO4 on the synthesis of CuBi2O4 microstructures was investigated. The samples were characterized by powder x-ray diffraction (XRD), scanning electron microscopy (SEM), Brunauer-Emmett-Teller (BET) analysis, x-ray photoelectron spectroscopy (XPS) and ultraviolet (UV)-visible diffuse reflectance spectroscopy. It is demonstrated that the use of KH2PO4 leads to the production of highly uniform CuBi2O4 microspheres hierarchically self-assembled by nanoparticles. With increasing the KH2PO4 concentration from 0.5 M to 1.4 M, the average diameter of the resultant microspheres decreases gradually from 3.3 μm to 1.4 μm. However, further increase in the KH2PO4 concentration up to 1.5 M leads to a sudden increase in the average diameter of the resultant microspheres up to 2.3 μm. In addition, a minor amount of bamboo leaf- or pine needle-like structures are visible in the samples prepared at the KH2PO4 concentrations of 1.0-1.5 M. The bandgap energy of the as-prepared samples is measured to be 1.89 eV by UV-visible diffuse reflectance spectroscopy. The electrochemical performance of the samples was investigated by cyclic voltammetry, galvanostatic charge-discharge measurements, and electrochemical impedance spectroscopy in 2 M KOH electrolyte. Among the hierarchical microspheres, those prepared at the KH2PO4 concentration of 1.4 M deliver a relatively higher specific capacitance due to their smaller size (1284 F g-1 at a current density of 2 A g-1).

  7. 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.

  8. 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

    2014-05-21

    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 × 10(3) S m(-1)), specific surface area (1258 m(2) 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

  9. Shape-controlled synthesis of Au@Pd core-shell nanoparticles and their corresponding electrochemical properties

    KAUST Repository

    Song, Hyon Min

    2012-01-01

    The shape-controlled synthesis of Au@Pd core-shell nanoparticles (NPs) was successfully achieved through the emulsion phase generated during the phase transfer from organic to aqueous medium. Contrary to conventional epitaxial growth for obtaining core-shell structures, this method does not require high temperatures and does not have shape restrictions. © 2012 The Royal Society of Chemistry.

  10. Electrochemical synthesis of one-dimensional ZnO nanostructures on ZnO seed layer for DSSC applications

    Science.gov (United States)

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

    2018-01-01

    Electrochemical deposition of vertically aligned zinc oxide (ZnO) nanorods were prepared on ZnO seeded fluorine doped tin oxide (FTO) substrate in the solutions consisting of different concentrations of hexamethylenetetramine (HMTA). The electrochemical, structural, morphological, vibrational and optical properties were characterized by cyclic voltammetry (CV), X-ray diffraction (XRD), scanning electron microscope (SEM), Raman spectroscopy and photoluminescence (PL) spectroscopy, respectively. CV curves confirm that metallic zinc phase is not deposited as the HMTA concentration is about 9 mM in a deposition solution. XRD patterns of the as-prepared films show that the increasing HMTA concentrations from 0 mM to 9 mM not only increase the formation of zinc hydrate chloride (Zn5(OH)8Cl2·H2O) but also decrease and finally disappear the metallic Zn deposition. After the as-prepared films annealed at 450 ° C, the crystalline phases of Zn and Zn5(OH)8Cl2·H2O are completely converted to ZnO hexagonal wurtzite phase with high intense growth (002) plane orientation. SEM images support that the vertical growth of ZnO nanostructures (nanorods and petals) with a few flowers is found to be in the cordillera structure as the films are deposited in the solutions consisting of 3 mM, 6 mM and 9 mM HMTA respectively. Raman and PL spectra confirm that the ZnO film deposited in the solution consisting of 9 mM HMTA has a higher crystalline nature with lesser atomic defects and is also higher c-axis growth than that of other films deposited in the solutions consisting of 0 mM, 3 mM and 6 mM, respectively. UV-vis absorbance spectra corroborate that the ZnO film deposited in the solution consisting of 9 mM HMTA shows a high dye absorbance as compared with other films. The efficiency of DSSCs based on ZnO photoanodes deposited in the solutions consisting of 0 mM and 9 mM HMTA was 1.79 and 3.75%, respectively. Electrochemical impedance spectra revealed that DSSC based on ZnO photoanode

  11. Synthesis, Characterizations and Investigation of Electrochemical Behaviours of 4-[(2-Hydroxyphenyliminomethyl]benzene-1,3-diol

    Directory of Open Access Journals (Sweden)

    Aysen D. Mulazimoglu

    2009-01-01

    Full Text Available This Schiff base ligand, 4-[(2-hydroxyphenylimino methyl]benzene-1,3-diol (HIBD was synthesized by reaction of 2-aminophenol and 2,4-dihydroxybenzaldehyde. The ligand was characterized by elemental analysis, FT-IR and 1H-NMR. Electrochemical behaviors were investigated on the glassy carbon electrode (GC surface with cyclic voltammetry (CV. The modification of HIBD on the GC was performed in +0.3 V and +2,8 V potential range using 100 mV s-1 scanning rate having 5 cycle. For the characterization of the modified surfaces 1 mM ferrocene redox probe in 0,1 M tetrabutylammonium tetrafluoroborate (TBATFB and 1 mM ferricyanide redox probe in 0.1 M H2SO4 were used.

  12. Well-integrated ZnO nanorod arrays on conductive textiles by electrochemical synthesis and their physical properties

    Science.gov (United States)

    Ko, Yeong Hwan; Kim, Myung Sub; Park, Wook; Yu, Jae Su

    2013-01-01

    We reported well-integrated zinc oxide (ZnO) nanorod arrays (NRAs) on conductive textiles (CTs) and their structural and optical properties. The integrated ZnO NRAs were synthesized by cathodic electrochemical deposition on the ZnO seed layer-coated CT substrate in ultrasonic bath. The ZnO NRAs were regularly and densely grown as well as vertically aligned on the overall surface of CT substrate, in comparison with the grown ZnO NRAs without ZnO seed layer or ultrasonication. Additionally, their morphologies and sizes can be efficiently controlled by changing the external cathodic voltage between the ZnO seed-coated CT substrate and the counter electrode. At an external cathodic voltage of -2 V, the photoluminescence property of ZnO NRAs was optimized with good crystallinity and high density.

  13. Facile synthesis of mesoporous NiO nanoflakes on graphene foam and its electrochemical properties for supercapacitor application

    Science.gov (United States)

    Lv, Jinlong; Wang, Zhuqing; Miura, Hideo

    2018-01-01

    Many NiO platelets were formed on Ni foam after hydrothermal process, while flower-like NiO with many small mesoporous nanoflakes was obtained on the surface of graphene foam. Electrochemical results showed that the NiO/graphene composites exhibited very high specific capacitance 1062 F g-1 at 1 A g-1 and excellent cycling stability (90.6% capacitance retention after 5000 cycles at 1 A g-1). The promising NiO/graphene composites exhibited higher supercapacitor performance than NiO platelets on Ni foam. The excellent supercapacitor performance of the former should be attributed to the 3D graphene conductive network and the mesoporous NiO nanoflakes which promoted efficient charge transport and electrolyte diffusion.

  14. 3D nitrogen-doped graphene aerogel nanomesh: Facile synthesis and electrochemical properties as the electrode materials for supercapacitors

    Science.gov (United States)

    Su, Xiao-Li; Fu, Lin; Cheng, Ming-Yu; Yang, Jing-He; Guan, Xin-Xin; Zheng, Xiu-Cheng

    2017-12-01

    Nitrogen-doped graphene aerogel nanomesh (N-GANM) has been hydrothermally prepared from graphene oxide and ammonium hydroxide using iron nitrate as the etching agent. The results showed that N-GANM with an interesting nanomesh structure on the graphene sheets maintained the 3D architecture of graphene aerogel (GA). Furthermore, it exhibited excellent electrochemical capacitive behavior and the specific capacitance value (290.0 F g-1 at 1 A g-1) remained approximately 90.3% after 2000 cycles in the three-electrode system. In addition, N-GANM displayed an energy density of 30.9 Wh kg-1 at the power density of 450.3 W kg-1 and excellent cycling stability retention (98%) after 10,000 cycles in the two-electrode symmetric device. The resulting N-GANM was expected to be a much favorable supercapacitor electrode material due to the heteroatom-doping and its unique porous structure.

  15. Synthesis of {beta}-MoO{sup 3} by vacuum drying and its structural and electrochemical characterisation

    Energy Technology Data Exchange (ETDEWEB)

    Juarez Ramirez, I.; Martinez-de la Cruz, A. [Centro de Investigacion y Desarrollo de Materiales Ceramicos (CIDEMAC), Facultad de Ciencias Quimicas, Universidad Autonoma de Nuevo Leon, Apartado Postal 1864, Monterrey, N.L. (Mexico)

    2003-01-01

    The {beta}-MoO{sub 3} was obtained successfully free of {alpha}-MoO{sub 3} through soft chemistry methods. The formation of {beta}-MoO{sub 3} with high purity was determined by the formation of the precursor MoO{sub 3}{center_dot}2H{sub 2}O when a solution of Na{sub 2}MoO{sub 4}{center_dot}2H{sub 2}O was passed through a cation-exchange resin. A structural, spectroscopic and thermal study of the polymorph synthesised was made by XRD, electron dispersion spectroscopy (EDS), FTIR and TGA/DTA techniques, respectively, in order to make a study about the possibilities of {beta}-MoO{sub 3} as active material in a lithium battery. Electrochemical experiments showed a high ability of the {beta}-MoO{sub 3} to form lithium molybdenum bronzes via a lithium insertion reaction.

  16. Pt-Fe catalyst nanoparticles supported on single-wall carbon nanotubes: Direct synthesis and electrochemical performance for methanol oxidation

    Science.gov (United States)

    Ma, Xiaohui; Luo, Liqiang; Zhu, Limei; Yu, Liming; Sheng, Leimei; An, Kang; Ando, Yoshinori; Zhao, Xinluo

    2013-11-01

    Single-wall carbon nanotubes (SWCNTs) supported Pt-Fe nanoparticles have been prepared by one-step hydrogen arc discharge evaporation of carbon electrode containing both Pt and Fe metal elements. The formation of SWCNTs and Pt-Fe nanoparticles occur simultaneously during the evaporation process. High-temperature hydrogen treatment and hydrochloric acid soaking have been carried out to purify and activate those materials in order to obtain a new type of Pt-Fe/SWCNTs catalyst for methanol oxidation. The Pt-Fe/SWCNTs catalyst performs much higher electrocatalytic activity for methanol oxidation, better stability and better durability than a commercial Pt/C catalyst according to the electrochemical measurements, indicating that it has a great potential for applications in direct methanol fuel cells.

  17. Facile electrochemical-assisted synthesis of TiO2 nanotubes and their role in Schottky barrier diode applications

    Science.gov (United States)

    Yilmaz, Mehmet; Cirak, Burcu Bozkurt; Aydogan, Sakir; Grilli, Maria Luisa; Biber, Mehmet

    2018-01-01

    Highly ordered TiO2 nanotube arrays were fabricated by electrochemical anodization of Ti foils. XRD measurements confirmed that properties of nanotube arrays belong to mixed anatase and rutile TiO2 phases with tetragonal crystal structure. Inter planar distance values of TiO2 nanotubes were determined with respect to Miller indices and varied from 0.16695 to 0.35339 nm. Furthermore, a Schottky diode made by Ag/TiO2 nano tube arrays/Ti was fabricated and current-voltage (I-V) characteristics of the device were analyzed at room temperature to investigate device performance. Ideality factor and barrier height have been determined as 2.39 and 0.92 eV, respectively. Results have been discussed in details.

  18. Synthesis, crystal structure, antibacterial activities, and electrochemical studies of new N,N‧-polymethylene bis-sulfonamides

    Science.gov (United States)

    Özbek, Neslihan; Alyar, Saliha; Mamaş, Serhat; Şahin, Ertan; Karacan, Nurcan

    2012-02-01

    Four disulfonamide derivatives (C2H5·SO2·NH)2(CH2)n (n = 2, 3, 4, 5) were synthesized and characterized by FTIR, 1H NMR, 13C NMR, HETCOR, LCMS and elemental analysis. Ethanesulfonamide-N,N'-pentamethylene bis was also characterized by X-ray single crystal diffraction measurement. The electrochemical characteristics of the disulfonamide derivatives were performed by cyclic voltammetry and chronoamperometry. 1H and 13C NMR chemical shifts of the compounds were calculated by using DFT/B3LYP methods with a 6-311++G (d,p) basis set. Antibacterial activity and the structural relationship of the compounds showed that activity decreases proportionately to the increasing length of the carbon chain between NH groups, log P values, hydration energy and molecular volumes. Anodic peak potentials and HOMO values do not correlate with the activity, but reduction potential and LUMO decrease weakly with increasing activity.

  19. Fabrication, Modification, and Emerging Applications of TiO2 Nanotube Arrays by Electrochemical Synthesis: A Review

    Directory of Open Access Journals (Sweden)

    Jian-Ying Huang

    2013-01-01

    Full Text Available Titania nanotube arrays (TNAs as a hot nanomaterial have a unique highly ordered array structure and good mechanical and chemical stability, as well as excellent anticorrosion, biocompatible, and photocatalytic performance. It has been fabricated by a facile electrochemical anodization in electrolytes containing small amounts of fluoric ions. In combination with our research work, we review the recent progress of the new research achievements of TNAs on the preparation processes, forming mechanism, and modification. In addition, we will review the potential and significant applications in the photocatalytic degradation of pollutants, solar cells, water splitting, and other aspects. Finally, the existing problems and further prospects of this renascent and rapidly developing field are also briefly addressed and discussed.

  20. Defective ZnCo2O4 with Zn vacancies: Synthesis, property and electrochemical application

    DEFF Research Database (Denmark)

    Huang, Guoyong; Yang, Yue; Sun, Hongyu

    2017-01-01

    . For the first time, the Zn0.95Co2O4 has been evaluated as an anode material for lithium-ion batteries. The Zn vacancies in defective ZnCo2O4 may decrease the probability of the reversible by-reaction between Zn and Li-Zn alloy by the cyclic voltammogram measurement. Compared to the traditional ZnCo2O4, the Zn...... vacancies in defective ZnCo2O4 can provide larger interface, activate more reaction sites and expand faster transport paths for both of Li-ions and electronics insertion/extraction, so the electrochemical performance of defective ZnCo2O4 has been enhanced highly. The discharge capacity retains at 652.2 m...

  1. Hydrothermal synthesis and electrochemical properties of Li₃V₂(PO₄)₃/C-based composites for lithium-ion batteries.

    Science.gov (United States)

    Sun, Chunwen; Rajasekhara, Shreyas; Dong, Youzhong; Goodenough, John B

    2011-09-01

    To improve performance at higher rates, we developed a hydrothermal method to prepare carbon-coated monoclinic lithium vanadium phosphate (Li(3)V(2)(PO(4))(3)) powder to be used as a cathode material for Li-ion batteries. The structural, morphological and electrochemical properties were characterized by X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM and TEM), and galvanostatic charge-discharge cycling. A superior cycle and rate behavior are demonstrated for Li(3)V(1.85)Sc(0.15)(PO(4))(3)/C and Li(2.96)Ca(0.02)V(2)(PO(4))(3)/C electrodes at charge-discharge current rates above 5C.

  2. Synthesis and electrochemical and in situ spectroelectrochemical characterization of manganese, vanadyl, and cobalt phthalocyanines with 2-naphthoxy substituents

    International Nuclear Information System (INIS)

    Ozcesmeci, Ibrahim; Koca, Atif; Guel, Ahmet

    2011-01-01

    Highlights: → Metallo (Mn, Co, VO) phthalocyanines bearing peripheral 2-naphthoxy-groups were synthesized by cyclotetramerisation of the corresponding phthalonitrile derivative. → Incorporation of the redox active metal ions into the phthalocyanine core extends the redox capabilities of the Pc ring. → The presence of O 2 in the electrolyte system influences both oxygen reduction reaction and the electrochemical and spectral behaviors of the complexes. → Homogeneous catalytic ORR process occurs via an 'inner sphere' chemical catalysis process. - Abstract: Metallo (Mn, Co, VO) phthalocyanines bearing peripheral 2-naphthoxy groups were synthesized by cyclotetramerisation of the corresponding phthalonitrile derivative. The phthalocyanine compounds were characterized by elemental analyses, mass, FT-IR and UV-vis spectral data. Three intense bands in the electronic spectra clearly indicate the absorptions resulting from naphthyl groups along with the Q and B bands of the phthalocyanines. Electrochemical and spectroelectrochemical measurements exhibit that incorporation of redox active metal ions, Co II and Mn III , into the phthalocyanine core extends the redox capabilities of the Pc ring including the metal-based reduction and oxidation couples of the metal. Presence of molecular oxygen in the electrolyte system affects the voltammetric and spectroelectrochemical responses of the cobalt and manganese phthalocyanines due to the interaction between the complexes and molecular oxygen. Interaction reaction of oxygen with CoPc occurs via an 'inner sphere' chemical catalysis process. While CoPc gives the intermediates [O 2 - -Co II Pc -2 ] - and [O 2 2 -Co II Pc -2 ] 2- , MnPc forms μ-oxo MnPc species. An in situ electrocolorimetric method has been applied to investigate the color of the electro-generated anionic and cationic forms of the complexes for possible electrochromatic applications.

  3. Synthesis and electrochemical characterization of myoglobin-antibody protein immobilized self-assembled gold nanoparticles on ITO-glass plate

    Energy Technology Data Exchange (ETDEWEB)

    Rajesh, E-mail: rajesh_csir@yahoo.com [Polymer and Soft Material Section, National Physical Laboratory (Council of Scientific and Industrial Research), Dr. K.S. Krishnan Road, New Delhi 110012 (India); Sharma, Vikash; Mishra, Sujeet K.; Biradar, Ashok M. [Polymer and Soft Material Section, National Physical Laboratory (Council of Scientific and Industrial Research), Dr. K.S. Krishnan Road, New Delhi 110012 (India)

    2012-01-16

    Highlights: Black-Right-Pointing-Pointer The Mb-Ab was covalently bonded to carboxyl groups of the mixed MUA and MPA over self-assembled GNPs. Black-Right-Pointing-Pointer This assembly on ITO-glass plate was used as an impedimetric immunosensor for myoglobin detection. Black-Right-Pointing-Pointer High loading of Mb-Ab, on the GNPs results in a wide range of Mb-Ag detection from 0.01 {mu}g to 1.65 {mu}g mL{sup -1} Black-Right-Pointing-Pointer The simple method and wide range of Mb-Ag detection makes this advantageous over other methods. - Abstract: We report a protein immobilized self-assembled monolayer (SAM) of gold nanoparticles (GNPs) on indium-tin-oxide (ITO) coated glass plate. The protein-antibody, Mb-Ab, was covalently immobilized over the self-assembly of GNPs through a mixed SAM of 11-mercapto undecanoic acid (MUA) and 3-mercapto propionic acid (MPA) via carbodiimide coupling reaction using N-(3-dimethylaminopropyl)-N Prime -ethyl carbodiimide (EDC) and N-hydroxy succinimide (NHS). The whole assembly was constructed on 0.25 cm{sup 2} area of ITO-glass plate (Mb-Ab/MUA-MPA/GNPs/APTES/ITO-glass) and an impedimetric study was carried out for its application in myoglobin detection. This prototype assembly was characterized by scanning electron microscopy, atomic force microscopy and electrochemical techniques. The modified electrode showed an increased electron-transfer resistance on coupling with protein antigen, Mb-Ag, in the presence of a redox probe [Fe(CN){sub 6}]{sup 3-/4-}. Its exhibits an electrochemical impedance response to protein myoglobin-antigen, Mb-Ag, concentration in a linear range from 0.01 {mu}g to 1.65 {mu}g mL{sup -1} with a lowest detection limit of 1.4 ng mL{sup -1}.

  4. Cobalt and Vanadium Trimetaphosphate Polyanions: Synthesis, Characterization, and Electrochemical Evaluation for Non-aqueous Redox-Flow Battery Applications.

    Science.gov (United States)

    Stauber, Julia M; Zhang, Shiyu; Gvozdik, Nataliya; Jiang, Yanfeng; Avena, Laura; Stevenson, Keith J; Cummins, Christopher C

    2018-01-17

    An electrochemical cell consisting of cobalt ([Co II/III (P 3 O 9 ) 2 ] 4-/3- ) and vanadium ([V III/II (P 3 O 9 ) 2 ] 3-/4- ) bistrimetaphosphate complexes as catholyte and anolyte species, respectively, was constructed with a cell voltage of 2.4 V and Coulombic efficiencies >90% for up to 100 total cycles. The [Co(P 3 O 9 ) 2 ] 4- (1) and [V(P 3 O 9 ) 2 ] 3- (2) complexes have favorable properties for flow-battery applications, including reversible redox chemistry, high stability toward electrochemical cycling, and high solubility in MeCN (1.09 ± 0.02 M, [PPN] 4 [1]·2MeCN; 0.77 ± 0.06 M, [PPN] 3 [2]·DME). The [PPN] 4 [1]·2MeCN and [PPN] 3 [2]·DME salts were isolated as crystalline solids in 82 and 68% yields, respectively, and characterized by 31 P NMR, UV/vis, ESI-MS(-), and IR spectroscopy. The [PPN] 4 [1]·2MeCN salt was also structurally characterized, crystallizing in the monoclinic P2 1 /c space group. Treatment of 1 with [(p-BrC 6 H 4 ) 3 N] + allowed for isolation of the one-electron-oxidized spin-crossover (SCO) complex, [Co(P 3 O 9 ) 2 ] 3- (3), which is the active catholyte species generated during cell charging. The success of the 1-2 cell provides a promising entry point to a potential future class of transition-metal metaphosphate-based all-inorganic non-aqueous redox-flow battery electrolytes.

  5. 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

  6. Hierarchical Thin Film Architectures for Enhanced Sensor Performance: Liquid Crystal-Mediated Electrochemical Synthesis of Nanostructured Imprinted Polymer Films for the Selective Recognition of Bupivacaine

    Directory of Open Access Journals (Sweden)

    Subramanian Suriyanarayanan

    2014-04-01

    Full Text Available Nanostructured bupivacaine-selective molecularly imprinted 3-aminophenylboronic acid-p-phenylenediamine co-polymer (MIP films have been prepared on gold-coated quartz (Au/quartz resonators by electrochemical synthesis under cyclic voltammetric conditions in a liquid crystalline (LC medium (triton X-100/water. Films prepared in water and in the absence of template were used for control studies. Infrared spectroscopic studies demonstrated comparable chemical compositions for LC and control polymer films. SEM studies revealed that the topologies of the molecularly imprinted polymer films prepared in the LC medium (LC-MIP exhibit discernible 40 nm thick nano-fiber structures, quite unlike the polymers prepared in the absence of the LC-phase. The sensitivity of the LC-MIP in a quartz crystal microbalance (QCM sensor platform was 67.6 ± 4.9 Hz/mM under flow injection analysis (FIA conditions, which was ≈250% higher than for the sensor prepared using the aqueous medium. Detection was possible at 100 nM (30 ng/mL, and discrimination of bupivacaine from closely related structural analogs was readily achieved as reflected in the corresponding stability constants of the MIP-analyte complexes. The facile fabrication and significant enhancement in sensor sensitivity together highlight the potential of this LC-based imprinting strategy for fabrication of polymeric materials with hierarchical architectures, in particular for use in surface-dependent application areas, e.g., biomaterials or sensing.

  7. Graphene quantum dots decorated with magnetic nanoparticles: Synthesis, electrodeposition, characterization and application as an electrochemical sensor towards determination of some amino acids at physiological pH

    International Nuclear Information System (INIS)

    Hasanzadeh, Mohammad; Karimzadeh, Ayub; Shadjou, Nasrin; Mokhtarzadeh, Ahad; Bageri, Leyla; Sadeghi, Sattar; Mahboob, Soltanali

    2016-01-01

    This study reports on the synthesis and characterization of a novel nano-composite, Fe 3 O 4 magnetic nanoparticles/graphene quantum dots (Fe 3 O 4 MNP-GQDs), for sensing of some amino acids. For the first time, as-synthesized GQDs and Fe 3 O 4 MNPs-GQDs was electrodeposited on the glassy carbon electrode (GCE) by cyclic voltammetry (CV) regime in the potential range from − 1.0 to 1.0 V. Fe 3 O 4 MNP-GQDs is engineered to specifically and effectively capture and enhancement the electrochemical signals of some amino acids at physiological pH due to the synergy among GQDs and magnetic nanoparticles. We have illustrated that the obtained Fe 3 O 4 MNPs-GQDs exhibited a much higher electroactivity individual GQDs and Fe 3 O 4 MNPs for the electrooxidation and detection of amino acid which was about 10 fold higher than for GQDs. Magnetic and specific properties of the Fe 3 O 4 MNP-GQDs can be exploited to capture and pre-concentration the amino acids onto its surface, which are important for detection of multi-amino acids. - Highlights: • Electrooxidation of amino acids was performed using Fe 3 O 4 MNP-GQDs. • Modified electrode shows new advantages as an amino acids sensor. • Excellent electrocatalytic activity was obtained for amino acids oxidation.

  8. 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.

  9. One-step electrochemical synthesis of 6-amino-4-hydroxy-2-napthalene-sulfonic acid functionalized graphene for green energy storage electrode materials

    Science.gov (United States)

    Kuila, Tapas; Khanra, Partha; Kim, Nam Hoon; Kuk Choi, Sung; Yun, Hyung Joong; Lee, Joong Hee

    2013-09-01

    A green approach for the one-step electrochemical synthesis of water dispersible graphene is reported. An alkaline solution of 6-amino-4-hydroxy-2-naphthalene-sulfonic acid (ANS) serves the role of electrolyte as well as surface modifier. High-purity graphite rods are used as electrodes which can be exfoliated under a constant electrical potential (˜20 V) to form ANS functionalized graphene (ANEG). The aqueous dispersion of ANEG obeyed Beer’s law at moderate concentrations, as evidenced from ultraviolet-visible spectroscopy analysis. X-ray diffraction analysis suggests complete exfoliation of graphite into graphene. Fourier transform infrared and x-ray photoelectron spectroscopy not only confirm the functionalization of graphene with ANS, but also suggest the formation of oxygen containing functional groups on the surface of ANEG. Raman spectra analysis indicates the presence of defects in ANEG as compared to pure graphite. Cyclic voltammetry and charge-discharge measurements of ANEG using three electrode systems show a specific capacitance of 115 F g-1 at a current density of 4 A g-1. The ANEG electrode exhibits 93% retention in specific capacitance after 1000 charge-discharge cycles, confirming its utility as a green energy storage electrode material.

  10. Push-pull D-π-Ru-π-A chromophores: synthesis and electrochemical, photophysical and second-order nonlinear optical properties.

    Science.gov (United States)

    Durand, Raphaël J; Gauthier, Sébastien; Achelle, Sylvain; Groizard, Thomas; Kahlal, Samia; Saillard, Jean-Yves; Barsella, Alberto; Le Poul, Nicolas; Le Guen, Françoise Robin

    2018-02-21

    The present work describes the one-pot synthesis and electrochemical, photophysical and second-order nonlinear optical (NLO) properties of a series of dipolar π-delocalized Ru(ii) dialkynyl complexes. The eight new asymmetrical D-π-Ru-π-A push-pull chromophores incorporate pyranylidene ligands as pro-aromatic donor groups (D) and formaldehyde, indane-1,3-dione, pyrimidine or pyrimidinium as electron-attracting groups (A) separated by ruthenium bis-acetylide fragments and π-conjugated linkers. The second-order nonlinear optical (NLO) properties of all eight complexes were determined by the Electric-Field-Induced Second Harmonic generation (EFISH) technique (operating at 1907 nm), and were compared to those of their purely organic analogs. All investigated compounds (organic and organometallic) exhibited positive μβ values, which dramatically increased for the complexes due to the presence of ruthenium in the π-conjugated core. The second-order NLO response could also be easily modulated by changing the nature of alkynyl substituents. The most promising ruthenium complexes 7 and 8 of the series with the pyrimidinium fragment displayed μβ values of 14 000 × 10 -48 esu. The effect of structural modifications on the redox and spectroscopic properties of the complexes was also studied. The intramolecular charge transfer (ICT) occurring through the ruthenium center of the push-pull σ-dialkynyl complexes was investigated by combining experimental and theoretical data.

  11. 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)

  12. A New All-Solid-State Hyperbranched Star Polymer Electrolyte for Lithium Ion Batteries: Synthesis and Electrochemical Properties

    International Nuclear Information System (INIS)

    Wang, Ailian; Xu, Hao; Zhou, Qian; Liu, Xu; Li, Zhengyao; Gao, Rui; Wu, Na; Guo, Yuguo; Li, Huayi; Zhang, Liaoyun

    2016-01-01

    Highlights: • A new hyperbranched multi-arm star polymer was successfully synthesized. • The star polymer electrolyte has good thermal stability and forming-film property. • The ion conductivity electrolyte can reach 8.3 × 10 −5 S cm −1 at room temperature. • The star polymer electrolyte has wide electrochemical windows of 4.7 V. - Abstract: A new hyperbranched multi-arm star polymer with hyperbranched polystyrene (HBPS) as core and polymethyl methacrylate-block-poly(ethylene glycol) methyl ether methacrylate(PMMA-b-PPEGMA) as arms was firstly synthesized by atom transfer radical polymerization. The obtained hyperbranched multi-arm star polymer (HBPS-(PMMA-b-PPEGMA) x ) exhibited good thermal stability with a thermal decomposition temperature of 372 °C. The transparent, free-standing, flexible polymer electrolyte film of the blending of HBPS-(PMMA-b-PPEGMA) x and lithium bis(trifluoromethanesulfonyl) imide (LiTFSI) was successfully fabricated by a solution casting method. The ionic conductivity of the hyperbranched star polymer electrolyte with a molar ratio of [EO]/[Li] of 30 could reach 8.3 × 10 −5 S cm −1 at 30 °C (with the content of PPEGMA of 83.7%), and 2.0 × 10 −4 S cm −1 at 80 °C (with the content of PPEGMA of 51.6%). The effect of the concentration of lithium salts on ionic conductivity was also investigated. The obtained all-solid-state polymer electrolyte possessed a wide electrochemical stability window of 4.7 V (vs. Li + /Li), and a lithium-ion transference number (t Li + ) up to 0.31. The interfacial impedance of the fabricated LiÔöépolymer electrolyteÔöéLi symmetric cell based on hyperbranched star multi-arm polymer electrolyte exhibited good interfacial compatibility between all-solid-state polymer electrolyte and electrodes. The excellent properties of the hyperbranched star polymer electrolyte made it attractive as solid-state polymer electrolyte for lithium-ion batteries.

  13. Synthesis and electrochemical properties of high performance polyhedron sphere like lithium manganese oxide for lithium ion batteries

    International Nuclear Information System (INIS)

    Guo, Donglei; Wei, Xiuge; Chang, Zhaorong; Tang, Hongwei; Li, Bao; Shangguan, Enbo; Chang, Kun; Yuan, Xiao-Zi; Wang, Haijiang

    2015-01-01

    Graphical abstract: Polyhedron structured sphere-like LiMn 2 O 4 synthesized from β-MnO 2 nanorod precursor via a solid state reaction at a temperature of 800 °C exhibits excellent rate capability and cycling performance at both 25 °C and 55 °C. - Highlights: • Polyhedron sphere-like LiMn 2 O 4 was synthesized from β-MnO 2 nanorod precursor. • The polyhedron sphere-like LiMn 2 O 4 exhibits excellent rate capability and cycling performance. • The polyhedron sphere-like structure spinel LiMn 2 O 4 suppresses the dissolution of manganese ions. • The polyhedron sphere-like LiMn 2 O 4 has high diffusion coefficient of Li + . - Abstract: Polyhedron structured sphere-like lithium manganese oxide (LiMn 2 O 4 ) is successfully synthesized from β-MnO 2 nanorod precursor via a solid state reaction at a temperature of 800 °C. For comparison, LiMn 2 O 4 materials with nanorod and octahedron structures are also obtained from β-MnO 2 nanorod precursor at temperatures of 700 °C and 900 °C, respectively. The galvanostatic charge–discharge result shows that the polyhedron sphere-like LiMn 2 O 4 sample exhibits the best electrochemical performance at high rate and high temperature. After 100 cycles at 5 C, this electrode is able to maintain 94% of its capacity at 25 °C and 81% at 55 °C. This is attributed to that the polyhedron sphere-like spinel LiMn 2 O 4 can suppress the dissolution of manganese ions. Based on Brunauer Emmett Teller (BET), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS), the polyhedron sphere-like LiMn 2 O 4 sample has the lowest BET surface area, largest diffusion coefficient of Li + and least charge transfer resistance. This study provides an insight into the capacity fading of LiMn 2 O 4 electrodes and the polyhedron structured sphere-like LiMn 2 O 4 can be a promising material for lithium ion batteries

  14. Controllable synthesis and enhanced electrochemical properties of multifunctional Au(core)Co(3)O(4shell) nanocubes.

    Science.gov (United States)

    Hu, Jianqiang; Wen, Zhenhai; Wang, Qiang; Yao, Xin; Zhang, Qian; Zhou, Jianhua; Li, Jinghong

    2006-12-07

    Multifunctional Au(core)Co(3)O(4shell) nanocubes were synthesized through the introduction of chloroauric acid (HAuCl(4)) into a typical hydrothermal system after a solvothermal process was completed to form metastable Co(3)O(4) hollow nanospheres in the presence of sodium dodecyl benzenesulfonate (SDBS), which served as the surfactant. The strategy suggested that HAuCl(4) played a vital role in the shape transformation and core/shell structure formation, and the sizes of the nanocubes can be tunable through control of the acid concentration. The core/shell structure of the nanocubes was demonstrated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and element analysis (EA) measurements. Moreover, Li ion battery measurement indicated that trace Au intercalation altered not only the size and shape of the Co(3)O(4) nanoparticles but also greatly increased their electrochemical properties. These multifunctional nanocubes will be not only helpful to study physical chemistry properties of magnetic nanocrystals but also are expected to find use in many fields such as biomolecular detection and analysis, sensor, electrochemistry, and Li ion batteries.

  15. Electrochemical synthesis of p-Cu{sub 2}O/n-ZnO nanorods hetero-junction for photovoltaic application

    Energy Technology Data Exchange (ETDEWEB)

    Rokade, A. V.; Rondiya, S. R.; Jadhavar, A. A.; Pandharkar, S. M.; Karpe, S. D.; Diwate, K. D. [School of Energy Studies, Savitribai Phule Pune University, Pune 411007 (India); Jadkar, S. R., E-mail: sandesh@physics.unipune.ac.in [Department of Physics, Savitribai Phule Pune University, Pune 411007 (India)

    2016-04-13

    Development of high performance visible light responsive solar cell materials has attracted wide interest due to their potential applications in the energy industries. In this work, ZnO nanorods films were successfully prepared on the ITO coated glass substrates via simple three electrode electrochemical deposition route. The Cu{sub 2}O nanoparticles were then electrodeposited on the surface of ZnO nanorods to form p-Cu{sub 2}O/n-ZnO core-shell hetero-structure. The synthesized ZnO, Cu{sub 2}O films and p-Cu{sub 2}O/n-ZnO hetero-structure were characterized by low angle x-ray diffraction, scanning electron microscopy, and UV-Visible spectrophotometer. Due to the hierarchical morphologies and core-shell structure, p-Cu{sub 2}O/n-ZnO hetero-structure shows a prominent visible-light-driven photocatalytic performance under the low intensity light irradiation. The obtained results suggest that it is possible to synthesize ZnO nanorods, Cu{sub 2}O films and p-Cu{sub 2}O/n-ZnO core-shell hetero-structure by a simple, cost effective and environment friendly electrodeposition process which can be useful for water splitting and solar cell device fabrication.

  16. Electrochemical synthesis of p-Cu2O/n-ZnO nanorods hetero-junction for photovoltaic application

    Science.gov (United States)

    Rokade, A. V.; Rondiya, S. R.; Jadhavar, A. A.; Pandharkar, S. M.; Karpe, S. D.; Diwate, K. D.; Jadkar, S. R.

    2016-04-01

    Development of high performance visible light responsive solar cell materials has attracted wide interest due to their potential applications in the energy industries. In this work, ZnO nanorods films were successfully prepared on the ITO coated glass substrates via simple three electrode electrochemical deposition route. The Cu2O nanoparticles were then electrodeposited on the surface of ZnO nanorods to form p-Cu2O/n-ZnO core-shell hetero-structure. The synthesized ZnO, Cu2O films and p-Cu2O/n-ZnO hetero-structure were characterized by low angle x-ray diffraction, scanning electron microscopy, and UV-Visible spectrophotometer. Due to the hierarchical morphologies and core-shell structure, p-Cu2O/n-ZnO hetero-structure shows a prominent visible-light-driven photocatalytic performance under the low intensity light irradiation. The obtained results suggest that it is possible to synthesize ZnO nanorods, Cu2O films and p-Cu2O/n-ZnO core-shell hetero-structure by a simple, cost effective and environment friendly electrodeposition process which can be useful for water splitting and solar cell device fabrication.

  17. One-pot synthesis of powder-form {beta}-Ni(OH){sub 2} monolayer nanosheets with high electrochemical performance

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Minmin; Ren, Wanzhong; Zhao, Yunan; Liu, Yan; Cui, Hongtao, E-mail: htcui@ytu.edu.cn [Yantai University, Shandong Provincial Engineering Research Center for Light Hydrocarbon Comprehensive Utilization, College of Chemistry and Chemical Engineering (China)

    2013-08-15

    In this work, {beta}-Ni(OH){sub 2} monolayer nanosheets, which had been thought to be unachievable, were successfully prepared for the first time by a one-pot strategy using epoxide as precipitation agent and sodium dodecyl sulfate (SDS) as surfactant. The characterization results indicate that the formation of monolayer morphology depends on the mediation of SDS molecules. The XRD patterns demonstrate the loose and defective packing of Ni(OH){sub 2} layers in the SDS intercalated samples. The disappearing of vibration band of free hydroxyl groups in the FTIR spectra suggests the interlayer separation resulted by SDS. The TEM and AFM images further confirm the formation of monolayer nanosheets. It is proposed that the in situ modification of the secondary growth unit of {beta}-Ni(OH){sub 2} by SDS allows its two-dimensional anisotropic growth through steric hindrance of SDS molecules. In addition, this effect allows isolation of {beta}-Ni(OH){sub 2} from solvent with keeping of monolayer nanosheet state in dry powder. The electrochemical measurement results indicate that {beta}-Ni(OH){sub 2} monolayer nanosheets own much higher urea electrolysis performance than their corresponding multilayer structure.

  18. Controllable Synthesis of Copper Oxide/Carbon Core/Shell Nanowire Arrays and Their Application for Electrochemical Energy Storage

    Directory of Open Access Journals (Sweden)

    Jiye Zhan

    2015-10-01

    Full Text Available Rational design/fabrication of integrated porous metal oxide arrays is critical for the construction of advanced electrochemical devices. Herein, we report self-supported CuO/C core/shell nanowire arrays prepared by the combination of electro-deposition and chemical vapor deposition methods. CuO/C nanowires with diameters of ~400 nm grow quasi-vertically to the substrates forming three-dimensional arrays architecture. A thin carbon shell is uniformly coated on the CuO nanowire cores. As an anode of lithium ion batteries, the resultant CuO/C nanowire arrays are demonstrated to have high specific capacity (672 mAh·g−1 at 0.2 C and good cycle stability (425 mAh·g−1 at 1 C up to 150 cycles. The core/shell arrays structure plays positive roles in the enhancement of Li ion storage due to fast ion/electron transfer path, good strain accommodation and sufficient contact between electrolyte and active materials.

  19. One-step hydrothermal synthesis of graphene decorated V2O5 nanobelts for enhanced electrochemical energy storage.

    Science.gov (United States)

    Lee, Minoh; Balasingam, Suresh Kannan; Jeong, Hu Young; Hong, Won G; Lee, Han-Bo-Ram; Kim, Byung Hoon; Jun, Yongseok

    2015-01-30

    Graphene-decorated V2O5 nanobelts (GVNBs) were synthesized via a low-temperature hydrothermal method in a single step. V2O5 nanobelts (VNBs) were formed in the presence of graphene oxide, a mild oxidant, which also enhanced the conductivity of GVNBs. From the electron energy loss spectroscopy analysis, the reduced graphene oxide (rGO) are inserted into the layered crystal structure of V2O5 nanobelts, which further confirmed the enhanced conductivity of the nanobelts. The electrochemical energy-storage capacity of GVNBs was investigated for supercapacitor applications. The specific capacitance of GVNBs was evaluated using cyclic voltammetry (CV) and charge/discharge (CD) studies. The GVNBs having V2O5-rich composite, namely, V3G1 (VO/GO = 3:1), showed superior specific capacitance in comparison to the other composites (V1G1 and V1G3) and the pure materials. Moreover, the V3G1 composite showed excellent cyclic stability and the capacitance retention of about 82% was observed even after 5000 cycles.

  20. Hydrothermal synthesis and electrochemical properties of nano-sized Co-Sn alloy anodes for lithium ion batteries

    International Nuclear Information System (INIS)

    He Jianchao; Zhao Hailei; Wang Jing; Wang Jie; Chen Jingbo

    2010-01-01

    Research highlights: → Nano-sized Co-Sn alloys were synthesized by hydrothermal route. → Li 2 O and CoSn can buffer the large volume change associated with lithiation of Sn. → A two-step reaction mechanism of CoSn 2 alloy during cycling was confirmed. - Abstract: Nano-sized Co-Sn alloys with a certain amount of Sn oxides used as potential anode materials for lithium ion batteries were synthesized by hydrothermal route. The effects of hydrothermal conditions and post annealing on the phase compositions and the electrochemical properties of synthesized powders were characterized by means of X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) with energy dispersive spectra (EDS) analysis and galvanostatic cycling tests. Prolonging the dwelling time at the same hydrothermal temperature can increase the content of Sn oxides, which will lead to a high initial irreversible capacity loss but a better cycling stability owing to the buffer effect of irreversible product Li 2 O. Heat-treatment can increase the crystallinity and cause the presence of a certain amount of inert CoSn component, which both have positive impact on the cycling stability of Co-Sn electrode. By comparison with the lithiation/delithiation processes of metal Sn, a two-step mechanism of CoSn 2 alloy during cycling was confirmed.

  1. Spontaneous Synthesis and Electrochemical Characterization of Nanostructured MnO2 on Nitrogen-Incorporated Carbon Nanotubes

    Directory of Open Access Journals (Sweden)

    Ying-Chu Chen

    2012-01-01

    Full Text Available This paper investigated the layered manganese dioxide with hydrate (MnO2⋅xH2O deposits onto nitrogen-containing carbon nanotube (CNxNTs as a hierarchical electrode for an energy-storage device. The dense and entangled CNxNTs were directly grown by microwave plasma-enhanced chemical vapor deposition (MPECVD on a carbon cloth (CC, and subsequently used as a current collector. By controlling the pH value of KMnO4 precursor solution, and incorporating nitrogen into CNTs as a reducing agent, the MnO2 thin layer was uniformly fabricated on the CNxNTs at room temperature by using a spontaneous reduction method. The role of incorporation nitrogen is not only capable of creating active sites on the CNT surface, but can also donate electrons to reduce MnO4- to MnO2 spontaneously. From the measurements of cyclic voltammograms and galvanostatic charge/discharge, MnO2/CNxNTs/CC composite electrodes illustrated excellent specific capacitance of 589.1 Fg-1. The key factor for high performance could be attributed to the thin-layered MnO2 nanostructure, which resulted in the full utilization of MnO2 deposits. Hence, the hierarchically porous MnO2/CNxNTs/CC electrodes exhibited excellent capacitive behavior for electrochemical capacitor application.

  2. Electrochemical synthesis of multi-armed CuO nanoparticles and their remarkable bactericidal potential against waterborne bacteria

    Science.gov (United States)

    Pandey, Pratibha; Merwyn, S.; Agarwal, G. S.; Tripathi, B. K.; Pant, S. C.

    2012-01-01

    Copper (II) oxide multi-armed nanoparticles composed of 500-1000 nm long radiating nanospicules with 100-200 nm width near the base and 50-100 nm width at the tapered ends and 25 nm thickness were synthesized by electrochemical deposition in the presence of an oxidant followed by calcination at 150 °C. The nanoparticles were characterized using SEM/EDX for morphology and composition, Raman spectroscopy for compound identification, and broth culture method for antibacterial efficacy. The CuO nanoparticles have shown remarkable bactericidal efficacy against Gram-positive and -negative waterborne disease causing bacteria like Escherichia coli, Salmonella typhi, s taphylococcus aureus and Bacillus subtilis. E. coli has been chosen as representative species for waterborne disease causing bacteria. In antibacterial tests 500 μg/mL nano CuO killed 3 × 108 CFU/mL E. coli bacteria within 4 h of exposure. Moreover, 8.3 × 106 CFU/mL E. coli were killed by 100 and 10 μg/mL nano CuO within 15 min and 4 h of exposure, respectively. Antibacterial activity of nano CuO has been found many-fold compared with commercial bulk CuO. The fate of nanoparticles after antibacterial test has also been studied. The synthesized CuO nanoparticles are expected to have potential antibacterial applications in water purification and in paints and coatings used on frequently touched surfaces and fabrics in hospital settings.

  3. A Novel Thiophene-Fused Polycyclic Aromatic with a Tetracene Core: Synthesis, Characterization, Optical and Electrochemical Properties

    Directory of Open Access Journals (Sweden)

    Yasushiro Nishioka

    2011-05-01

    Full Text Available FeCl3-mediated oxidative cyclization was successfully used to construct an extended thiophene-pendant pyrene skeleton and synthesize a novel thiophene-fused polycyclic aromatic (THTP-C with a tetracene core. The identity of the compound was confirmed by 1H-NMR, 13C-NMR, MS, and elemental analysis. Meanwhile, a single crystal of THTP-C was obtained and analyzed by X-ray single-crystal diffraction. THTP-C has a “saddle” shaped π-conjugated 1-D supramolecular structure, and favors highly ordered self-assembly by π-π interactions as evidenced by its concentration-dependent 1H-NMR spectra in solution. The optical properties of THTP-C were investigated by ultraviolet-visible (UV-Vis and photoluminescence (PL spectroscopy and its electrochemical properties were investigated by cyclic voltammetry (CV. The relatively large band gap (2.86 eV, low EHOMO level (−5.64 eV and intermolecular π-π interactions imply that THTP-C has a high stability against photo-degradation and oxidation, and may be a promising candidate for stable hole-transporting materials.

  4. Synthesis of bismuth (III oxide films based anodes for electrochemical degradation of reactive blue 19 and crystal violet

    Directory of Open Access Journals (Sweden)

    Petrović Milica M.

    2014-01-01

    Full Text Available The Bi2O3 films-based anodes were synthesized by electrodeposition of Bi on stainless steel substrate at constant current density and during different deposition times, fallowed by calcination, forming Bi2O3. The thickness of the films was determined by two methods: the observation under the microscope and by calculation from mass difference. Electrochemical proceses at the anodes were ivestigated by linear sweep voltammetry. At the anodes obtained within 2, 5, 10 and 15 minutes of deposition, two dyes, namely: Reactive Blue 19 and Crystal Violet, were decolorized by oxidation with •OH radical, generated from H2O2 decomposition at the anodes. Decoloration times of the anodes varied, and the shortest one was achieved with the anode obtained during 5 minutes of deposition, with the film thickness of 2.5±0.3 μm. The optimal H2O2 concentration for the dyes degradation was found to be 10 mmol dm-3. [Projekat Ministarstva nauke Republike Srbije, br. ТR 34008

  5. Controllable Synthesis of Copper Oxide/Carbon Core/Shell Nanowire Arrays and Their Application for Electrochemical Energy Storage.

    Science.gov (United States)

    Zhan, Jiye; Chen, Minghua; Xia, Xinhui

    2015-10-09

    Rational design/fabrication of integrated porous metal oxide arrays is critical for the construction of advanced electrochemical devices. Herein, we report self-supported CuO/C core/shell nanowire arrays prepared by the combination of electro-deposition and chemical vapor deposition methods. CuO/C nanowires with diameters of ~400 nm grow quasi-vertically to the substrates forming three-dimensional arrays architecture. A thin carbon shell is uniformly coated on the CuO nanowire cores. As an anode of lithium ion batteries, the resultant CuO/C nanowire arrays are demonstrated to have high specific capacity (672 mAh·g -1 at 0.2 C) and good cycle stability (425 mAh·g -1 at 1 C up to 150 cycles). The core/shell arrays structure plays positive roles in the enhancement of Li ion storage due to fast ion/electron transfer path, good strain accommodation and sufficient contact between electrolyte and active materials.

  6. Photoinduced interactions of supramolecular ruthenium(II) complexes with plasmid DNA: synthesis and spectroscopic, electrochemical, and DNA photocleavage studies.

    Science.gov (United States)

    Swavey, Shawn; DeBeer, Madeleine; Li, Kaiyu

    2015-04-06

    Two new bridging ligands have been synthesized by combining substituted benzaldehydes with phenanthrolinopyrrole (php), resulting in new polyazine bridging ligands. The ligands have been characterized by (1)H NMR, mass spectroscopy, and elemental analysis. These new ligands display π-π* transitions above 500 nm with modest molar absorptivities. Upon excitation at the ligand-centered charge-transfer transition, weak emission with a maximum wavelength of 612 nm is observed. When coordinated to two ruthenium(II) bis(bipyridyl) groups, the new bimetallic complexes generated give an overall 4+ charge. The electronic transitions of the bimetallic ruthenium(II) complexes display traditional π-π* transitions at 287 nm and metal-to-ligand charge-transfer transitions at 452 nm with molar absorptivities greater than 30000 M(-1) cm(-1). Oxidation of the ruthenium(II) metal centers to ruthenium(III) occurs at potentials above 1.4 V versus the Ag/AgCl reference electrode. Spectroscopic and electrochemical measurements indicate that the ruthenium(II) moieties behave independently. Both complexes are water-soluble and show the ability to photonick plasmid DNA when irradiated with low-energy light above 550 nm. In addition, one of the complexes, [Ru(bpy)2php]2Van(4+), shows the ability to linearize plasmid DNA and gives evidence, by gel electrophoresis, of photoinduced binding to plasmid DNA.

  7. Novel thiourea derivative and its complexes: Synthesis, characterization, DFT computations, thermal and electrochemical behavior, antioxidant and antitumor activities

    Science.gov (United States)

    Yeşilkaynak, Tuncay; Muslu, Harun; Özpınar, Celal; Emen, Fatih Mehmet; Demirdöğen, Ruken Esra; Külcü, Nevzat

    2017-08-01

    A novel thiourea derivative, N-((2-chloropyridin-3-yl)carbamothioyl) thiophene-2-carboxamide,C11H8ClN3OS2 (HL) and its Co(II), Ni(II) and Cu(II) complexes (ML2 type) were prepared and characterized by elemental analysis, FT-IR,1H NMR and HR-MS methods. The crystal structure of HL was also investigated by single crystal X-ray diffraction study. The HL crystallizes in the orthorhombic crystal system with P 21 21 21 space group, Z = 4, a = 3.8875(3) Å, b = 14.6442(13) Å, c = 21.8950(19) Å. The [ML2] complex structures were optimized by using B97D/TZVP level. Molecular orbitals of HL ligand were calculated at the same level. Thermal and electrochemical behaviors of the complexes were investigated. Anticancer and antioxidant activities of the complexes were also investigated. Antioxidant activities were determined by using DPPH (2,2-diphenyl-1-picrylhydrazyl) and ABTS (2,2‧-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) assays. Anticancer activities were studied via MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) assay in MCF-7 (Michigan Cancer Foundation-7) breast cancer cells.

  8. Controllable synthesis of hollow bipyramid β-MnO(2) and its high electrochemical performance for lithium storage.

    Science.gov (United States)

    Chen, Wei-Min; Qie, Long; Shao, Qing-Guo; Yuan, Li-Xia; Zhang, Wu-Xing; Huang, Yun-Hui

    2012-06-27

    Three types of MnO2 nanostructures, viz., α-MnO2 nanotubes, hollow β-MnO2 bipyramids, and solid β-MnO2 bipyramids, have been synthesized via a simple template-free hydrothermal method. Cyclic voltammetry and galvanostatic charge/discharge measurements demonstrate that the hollow β-MnO2 bipyramids exhibit the highest specific capacity and the best cyclability; the capacity retains 213 mAh g(-1) at a current density of 100 mA g(-1) after 150 cycles. XRD patterns of the lithiated β-MnO2 electrodes clearly show the expansion of lattice volume caused by lithiation, but the structure keeps stable during lithium insertion/extraction process. We suggest that the excellent performance for β-MnO2 can be attributed to its unique electrochemical reaction, compact tunnel-structure and hollow architecture. The hollow architecture can accommodate the volume change during charge/discharge process and improve effective diffusion paths for both lithium ions and electrons.

  9. Controllable Electrochemical Synthesis of Copper Sulfides as Sodium-Ion Battery Anodes with Superior Rate Capability and Ultralong Cycle Life.

    Science.gov (United States)

    Li, Haomiao; Wang, Kangli; Cheng, Shijie; Jiang, Kai

    2018-03-07

    Sodium-ion batteries (SIBs) are prospective alternative to lithium-ion batteries for large-scale energy-storage applications, owing to the abundant resources of sodium. Metal sulfides are deemed to be promising anode materials for SIBs due to their low-cost and eco-friendliness. Herein, for the first time, series of copper sulfides (Cu 2 S, Cu 7 S 4 , and Cu 7 KS 4 ) are controllably synthesized via a facile electrochemical route in KCl-NaCl-Na 2 S molten salts. The as-prepared Cu 2 S with micron-sized flakes structure is first investigated as anode of SIBs, which delivers a capacity of 430 mAh g -1 with a high initial Coulombic efficiency of 84.9% at a current density of 100 mA g -1 . Moreover, the Cu 2 S anode demonstrates superior capability (337 mAh g -1 at 20 A g -1 , corresponding to 50 C) and ultralong cycle performance (88.2% of capacity retention after 5000 cycles at 5 A g -1 , corresponding to 0.0024% of fade rate per cycle). Meanwhile, the pseudocapacitance contribution and robust porous structure in situ formed during cycling endow the Cu 2 S anodes with outstanding rate capability and enhanced cyclic performance, which are revealed by kinetics analysis and ex situ characterization.

  10. Low and High Molecular Mass Dithienopyrrole-Naphthalene Bisimide Donor-Acceptor Compounds: Synthesis, Electrochemical and Spectroelectrochemical Behaviour.

    Science.gov (United States)

    Rybakiewicz, Renata; Glowacki, Eric D; Skorka, Lukasz; Pluczyk, Sandra; Zassowski, Pawel; Apaydin, Dogukan Hazar; Lapkowski, Mieczyslaw; Zagorska, Malgorzata; Pron, Adam

    2017-02-24

    Two low molecular weight electroactive donor-acceptor-donor (DAD)-type molecules are reported, namely naphthalene bisimide (NBI) symmetrically core-functionalized with dithienopyrrole (NBI-(DTP) 2 ) and an asymmetric core-functionalized naphthalene bisimide with dithienopyrrole (DTP) substituent on one side and 2-ethylhexylamine on the other side (NBI-DTP-NHEtHex). Both compounds are characterized by low optical bandgaps (1.52 and 1.65 eV, respectively). NBI-(DTP) 2 undergoes oxidative electropolymerization giving the electroactive polymer of ambipolar character. Its two-step reversible reduction and oxidation is corroborated by complementary EPR and UV/Vis-NIR spectroelectrochemical investigations. The polymer turned out to be electrochemically active not only in aprotic solvents but also in aqueous electrolytes, showing a distinct photocathodic current attributed to proton reduction. Additionally, poly(NBI-(DTP) 2 ) was successfully tested as a photodiode material. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Synthesis and application of carbowax/polypyrrole nanocomposite for fabrication of electrochemical sensor to detect 2,4-DNT vapor

    Science.gov (United States)

    Foroutan Koudehi, Masoumeh; Mahdi Pourmortazavi, Seied

    2017-08-01

    In this study, an electrochemical sensor coated with carbowax/polypyrrole nanocomposite was fabricated so as to be sensitive to 2,4-dinitrotoluene (2,4-DNT) as a nitroaromatic explosive. The variation in electrical resistance was used as the mechanism by which the sensor responded to the concentration of explosive vapor. Polypyrrole (PPy) nanoparticles were synthesized and characterized using a scanning electron microscope (SEM), ATR-FTIR (attenuated total reflection Fourier transform infrared) spectroscopy and x-ray diffraction analysis (XRD). The results showed that the fabricated PPy nanoparticles have a near spherical morphology with an average size of around 56 nm. The surface of the sensor template was then coated with a layer of nanocomposite composed of the synthesized PPy nanoparticles and carbowax polymer. Calibration and performance testing of the fabricated sensors were carried out with a special setup designed for explosive vapor generation under static conditions. The developed sensor was able to sense different concentrations of the explosive (0.5-100 ppm). The coated sensor showed a linear response in the concentration range of 0.5-50 ppm. The results showed that the designed sensor had a favorable sensitivity to the explosive. The calibration curve and sensitivity of the fabricated carbowax/PPy sensor was also determined in the explosive vapor concentration range of 0.5-50 ppm of 2,4-DNT under static conditions.

  12. 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...

  13. Synthesis, photophysical and electrochemical properties, and protein-binding studies of luminescent cyclometalated iridium(III) bipyridine estradiol conjugates.

    Science.gov (United States)

    Lo, Kenneth Kam-Wing; Zhang, Kenneth Yin; Chung, Chi-Keung; Kwok, Karen Ying

    2007-01-01

    A new series of luminescent cyclometalated iridium(III) bipyridine estradiol conjugates [Ir(N-C)2(N-N)](PF6) (N-N = 5-(4-(17alpha-ethynylestradiolyl)phenyl)-2,2'-bipyridine, bpy-est, HN-C = 2-phenylpyridine, Hppy (1 a), 1-phenylpyrazole, Hppz (2 a), 7,8-benzoquinoline, Hbzq (3 a), 2-phenylquinoline, Hpq (4 a), 2-((1,1'-biphenyl)-4-yl)benzothiazole, Hbsb (5 a); N-N = 4-(N-(6-(4-(17alpha-ethynylestradiolyl)benzoylamino)hexyl)aminocarbonyl)-4'-methyl-2,2'-bipyridine, bpy-C6-est, HN-C = Hppy (1 b), Hppz (2 b), Hbzq (3 b), Hpq (4 b), Hbsb (5 b)) was synthesized, characterized, and their photophysical and electrochemical properties studied. Upon photoexcitation, all the complexes displayed intense and long-lived emission in fluid solutions at 298 K and in low-temperature glass. The emission of complexes 1 a-3 a and 1 b-3 b was assigned to a triplet metal-to-ligand charge-transfer ((3)MLCT) (dpi(Ir)-->pi*(bpy-est and N-C-)) state mixed with some triplet intraligand ((3)IL) (pi-->pi*) (N-C- and N-N) character. However, the emissive states of the pq- and bsb- complexes 4 a, 4 b, 5 a, and 5 b showed substantial (3)IL (pi-->pi*) (pq-/bsb-) character. The lipophilicity of all the complexes was determined by reversed-phase HPLC. Upon binding to estrogen receptor alpha, all of these iridium(III) estradiol conjugates exhibited emission enhancement and lifetime extension, rendering them a novel series of luminescent probes for this receptor.

  14. Synthesis, characterization and electrochemical studies of Pt- W/C catalyst for polymer electrolyte membrane fuel cells

    International Nuclear Information System (INIS)

    Ahmed, R.; Shahid, S.; Ansari, M. S.

    2013-01-01

    Pt-W/C catalyst was synthesized by slow reduction of platinum and tungsten solutions in the desired ratio with subsequent deposition on the Vulcan carbon already added to the solution. Crystallite size of catalyst was about 9 nm and its density, cell volume, d-spacing and lattice parameter were also calculated. EDX analysis of the catalyst was also done. Electrochemical surface area of the catalyst was determined by cyclic voltammetry (CV). CV of the catalyst was done both in acidic and basic media to find out the peak potential, peak current, specific activity and mass activity of the catalyst. Peak potential versus scan rate plots showed that the electro oxidation of methanol is an irreversible process. Tafel equation was used to plot polarization curves to find out the exchange current density. Higher values of exchange current indicate better catalysts. Specific activities of the catalyst were determined in acidic and basic media and it was found that the specific activity in basic media increased substantially as compared to acidic media. The specific activity in acidic media was 83 mA/mg pt whereas in basic media it was 137mA/mg pt which is a substantial increase. Heterogeneous rate constant in acidic media was 6.15 * 10-6 cm/ s and in basic media it was 4.92 * 10-5 cm/s which is much higher in basic media. In this binary catalyst addition of tungsten has increased the catalytic activity but it is non-noble metal thus will decrease the cost. Stability studies of the catalyst were done upto fifty cycles both in acidic and basic media and was found quite stable in both the media. (author)

  15. Synthesis, characterization and electrochemical studies of Pt-W/C catalyst for polymer electrolyte membrane fuel cells

    International Nuclear Information System (INIS)

    Ahmed, Riaz; Shahid, Saliha; Ansari, Muhammad Shahid

    2014-01-01

    Pt-W/C catalyst was synthesized by slow reduction of platinum and tungsten solutions in the desired ratio with subsequent deposition on the Vulcan carbon already added to the solution. Crystallite size of catalyst was about 9 nm and its density, cell volume, d-spacing and lattice parameter were also calculated. EDX analysis of the catalyst was also done. Electrochemical surface area of the catalyst was determined by cyclic voltammetry (CV). CV of the catalyst was done both in acidic and basic media to find out the peak potential, peak current, specific activity and mass activity of the catalyst. Peak potential versus scan rate plots showed that the electro oxidation of methanol is an irreversible process. Tafel equation was used to plot polarization curves to find out the exchange current density. Higher values of exchange current indicate better catalysts. Specific activities of the catalyst were determined in acidic and basic media and it was found that the specific activity in basic media increased substantially as compared to acidic media. The specific activity in acidic media was 83 mA/mg pt whereas in basic media it was 137mA/mg pt which is a substantial increase. Heterogeneous rate constant in acidic media was 6.15 x 10 −6 cm/ s and in basic media it was 4.92 x 10 −5 cm/s which is much higher in basic media. In this binary catalyst addition of tungsten has increased the catalytic activity but it is non-noble metal thus will decrease the cost. Stability studies of the catalyst were done upto fifty cycles both in acidic and basic media and was found quite stable in both the media

  16. Synthesis and electrochemical sodium and lithium insertion properties of sodium titanium oxide with the tunnel type structure

    Science.gov (United States)

    Kataoka, Kunimitsu; Akimoto, Junji

    2016-02-01

    Polycrystalline sample of sodium titanium oxide Na2Ti4O9 with the tunnel-type structure was prepared by topotactic sodium extraction in air atmosphere from the as prepared Na3Ti4O9 sample. The starting Na3Ti4O9 compound was synthesized by solid state reaction at 1273 K in Ar atmosphere. The completeness of oxidation reaction from Na3Ti4O9 to Na2Ti4O9 was monitored by the change in color from dark blue to white, and was also confirmed by the Rietveld refinement using the powder X-ray diffraction data. The sodium deficient Na2Ti4O9 maintained the original Na2.08Ti4O9-type tunnel structure and had the monoclinic crystal system, space group C2/m, and the lattice parameters of a = 23.1698(3) Å, b = 2.9406(1) Å, c = 10.6038(2) Å, β = 102.422(3)°, and V = 705.57(2) Å3. The electrochemical measurements of thus obtained Na2Ti4O9 sample showed the reversible sodium insertion and extraction reactions at 1.1 V, 1.5 V, and 1.8 V vs. Na/Na+, and reversible lithium insertion and extraction reactions at around 1.4 V, 1.8 V, and 2.0 V vs. Li/Li+. The reversible capacity for the lithium cell was achieved to be 104 mAh g-1 at the 100th cycle.

  17. New unsymmetrically benzene-fused bis (tetrathiafulvalene): synthesis, characterization, electrochemical properties and electrical conductivity of their materials.

    Science.gov (United States)

    Abbaz, Tahar; Bendjeddou, Amel; Gouasmia, Abdelkrim; Villemin, Didier; Shirahata, Takashi

    2014-03-17

    The synthesis of new unsymmetrically benzene-fused bis (tetrathiafulvalene) has been carried out by a cross-coupling reaction of the respective 4,5-dialkyl-1,3-dithiole-2-selenone 6-9 with 2-(4-(p-nitrophenyl)-1,3-dithiole-2-ylidene)-1,3,5,7-tetrathia-s-indacene-6-one 5 prepared by olefination of 4-(p-nitrophenyl)-1,3-dithiole-2-selenone 3 and 1,3,5,7-tetrathia-s-indacene-2,6-dione 4. The conversion of the nitro moiety 10a-d to amino 11a-d then dibenzylamine 12a-d groups respectively used reduction and alkylation methods. The electron donor ability of these new compounds has been measured by cyclic voltammetry (CV) technique. Charge transfer complexes with tetracyanoquino-dimethane (TCNQ) were prepared by chemical redox reactions. The complexes have been proven to give conducting materials.

  18. New Unsymmetrically Benzene-Fused Bis (Tetrathiafulvalene: Synthesis, Characterization, Electrochemical Properties and Electrical Conductivity of Their Materials

    Directory of Open Access Journals (Sweden)

    Tahar Abbaz

    2014-03-01

    Full Text Available The synthesis of new unsymmetrically benzene-fused bis (tetrathiafulvalene has been carried out by a cross-coupling reaction of the respective 4,5-dialkyl-1,3-dithiole-2-selenone 6–9 with 2-(4-(p-nitrophenyl-1,3-dithiole-2-ylidene-1,3,5,7-tetrathia-s-indacene-6-one 5 prepared by olefination of 4-(p-nitrophenyl-1,3-dithiole-2-selenone 3 and 1,3,5,7-tetrathia-s-indacene-2,6-dione 4. The conversion of the nitro moiety 10a–d to amino 11a–d then dibenzylamine 12a–d groups respectively used reduction and alkylation methods. The electron donor ability of these new compounds has been measured by cyclic voltammetry (CV technique. Charge transfer complexes with tetracyanoquino-dimethane (TCNQ were prepared by chemical redox reactions. The complexes have been proven to give conducting materials.

  19. Microwave-assisted one-pot synthesis of metal/metal oxide nanoparticles on graphene and their electrochemical applications

    International Nuclear Information System (INIS)

    Wang Shuangyin; Jiang San Ping; Wang Xin

    2011-01-01

    Graphical abstract: Display Omitted Research highlights: → Microwave polyol method is efficient to deposit nanoparticles on graphene. → SnO 2 /graphene is more efficient than graphene for supercapacitor. → PtRu/graphene is more active than commercial PtRu/C for methanol oxidation. - Abstract: An effective synthesis strategy of hybrid metal (PtRu)/metal oxide (SnO 2 ) nanoparticles on graphene nanocomposites is developed using a microwave-assisted one-pot reaction process. The mixture of ethylene glycol (EG) and water is used as both solvent and reactant. In the reaction system for the synthesis of SnO 2 /graphene nanocomposite, EG not only reduces graphene oxide (GO) to graphene, but also results in the formation of SnO 2 facilitated by the presence of a small amount of water. On the other hand, in the reaction system for preparation of PtRu/graphene nanocomposites, EG acts as solvent and reducing agent for reduction of PtRu nanoparticles from their precursors and reduction of graphene from graphene oxide. Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM) characterizations confirm the feasibility of the microwave-assisted reaction system to simultaneously reduce graphene oxide and to form SnO 2 or PtRu nanoparticles. The as-synthesized SnO 2 /graphene hybrid composites show a much higher supercapacitance than the pure graphene, and the as-prepared PtRu/graphene show much better electrocatalytic activity for methanol oxidation compared to the commercial E-TEK PtRu/C electrocatalysts.

  20. Electrochemical properties of dip-coated vanadium pentaoxide thin ...

    Indian Academy of Sciences (India)

    studied in 1 M NaNO3 electrolyte using cyclic voltammetery, electrochemical impedance spectroscopy and galvano- ... Chemical synthesis; annealing; thin films; electrochemical properties; energy storage. 1. Introduction. Supercapacitors or ... electrochemical characterizations of the prepared samples are investigated in 1 ...

  1. One pot synthesis of Cu2O/RGO composite using mango bark extract and exploration of its electrochemical properties

    International Nuclear Information System (INIS)

    Kumar, J. Sharath; Jana, Milan; Khanra, Partha; Samanta, Pranab; Koo, Hyeyoung; Murmu, Naresh Chandra; Kuila, Tapas

    2016-01-01

    Highlights: • Simultaneous bio-reduction of GO and CuSO 4 using mango bark extract is presented. • The sensitivity and the LoD for H 2 O 2 are found to be 7.435 μA μM −1 & 42.35 nM. • Specific capacitance of the asymmetric device is 195 F g −1 at 2 A g −1 . • Retention in specific capacitances is ∼79% after 5000 charge-discharge cycles. - Abstract: A facile and eco-friendly approach for the simultaneous reduction of graphene oxide (GO) as well as copper acetate to prepare Cu 2 O decorated reduced GO (RGO) has been demonstrated. Herein, an easily available and naturally occurring mango bark (M. indica) extract has been used as the reducing agent instead of hazardous and toxic chemicals. Fourier transform infrared and X-ray photoelectron spectroscopy have been performed to confirm the removal of oxygen functional groups from the surface of GO. X-ray diffraction pattern reveals the formation of Cu 2 O nanoparticles (NPs). Morphological characterization was carried out using field emission scanning electron and transmission electron microscopy to confirm the decoration of RGO with Cu 2 O NPs. The electrocatalytic behaviour of the RGO/Cu 2 O composite has been carried by cyclic voltammetry and amperometric analysis. It shows the utility of the RGO/Cu 2 O composite as an electrochemical sensor towards H 2 O 2 detection. The sensitivity and limit of detection for the composite are found to be 7.435 μA μM −1 & 42.35 nM, respectively. The RGO/Cu 2 O//RGO asymmetric supercapacitor device shows the specific capacitance (SC) of 195 F g −1 at a current density of 2 A g −1 and energy density of 37.7 Wh kg −1 with 79% retention in SC after 5000 charge-discharge cycles.

  2. Synthesis and electrochemical characterization of highly tolerant Pd electrocatalysts as cathodes in direct ethylene glycol fuel cells (DEGFC)

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez Varela, F.J.; Fraire Luna, S. [Cinvestav, Unidad Saltillo, Ramos Arizpe, Coahuila (Mexico)] e-mail: javier.varela@cinvestav.edu.mx; Savadogo, O. [Laboratoire d' Electrochimie et de Materiaux Energetiques, Ecole Polytechnique de Montreal, Montreal, QC (Canada)

    2009-09-15

    Highly selective Pd electrocatalysts were synthesized by the formic acid method and evaluated as cathodes for DEGFC applications. In rotating disc measurements in acid medium, the Pd/C cathode showed important catalytic activity for the Oxygen Reduction Reaction (ORR). In the presence of ethylene glycol (EG, C{sub 2}H{sub 6}O{sub 2}), Pd/C exhibited an excellent electrochemical behavior and full tolerance to the organic molecule. No current density peaks associated to the EG oxidation reaction emerged and the shift in onset potential for the ORR (Eonset) toward more negative potentials was negligible on this cathode. Moreover, the evaluation of Pd/C in a DEGFC operating at 80 degrees Celsius demonstrated its high performance as cathode. As a comparison, commercial Pt/C was tested under the same conditions showing a limited selectivity for the ORR. The detrimental effect of EG on the Pt electrocatalysts resulted in high intensity current density peaks due to the oxidation of EG and a significant shift in Eonset. Given these results, it is expected that highly efficient Pd-based cathodes can find application in DEGFCs. [Spanish] Se sintetizaron electrocatalizadores altamente selectivos mediante el metodo de acido formico y se evaluaron como catodos en aplicaciones de CCGED. En mediciones de disco rotatorio en medio acido, el catodo Pd/C mostro importante actividad catalitica en la reaccion de reduccion de oxigeno (RRO). En la presencia de glicol de etileno (GE, C{sub 2}H{sub 6}O{sub 2}), Pd/C exhibio un excelente comportamiento electromecanico y tolerancia total a la molecula organica. No surgieron picos de densidad de corriente asociados con la reaccion de oxidacion de GE y el corrimiento en el potencial de inicio para la RRO (Einicio) hacia potenciales mas negativos fue despreciable en este catodo. Como comparacion, se probo un Pt/C bajo las mismas condiciones y se observo una selectividad limitada para el RRO. El efecto perjudicial de GE en el electrocatalizador

  3. Synthesis, characterization and electrochemical properties of the V{sub 2}O{sub 5}.nH{sub 2}O/AlO(OH).nH{sub 2}O xerogel composite

    Energy Technology Data Exchange (ETDEWEB)

    Zampronio, Elaine C.; Oliveira, Herenilton P. [Universidade de Sao Paulo, Ribeirao Preto (SP) (Brazil). Departamento de Quimica - FFCLRP; Lassali, Tania A.F. [Universidade de Sao Paulo, Ribeirao Preto (SP) (Brazil). PCARP - Laboratorio de Residuos Quimicos

    2005-10-10

    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{sub 2}O{sub 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{sub 2}O{sub 5} xerogel dispersed in the alumina matrix is quite similar to that found for the V{sub 2}O{sub 5} xerogel alone and the inorganic matrix leads to stabilization of V{sub 2}O{sub 5} xerogel structure. (author)

  4. Synthesis, characterization, and electrochemical performance of nitrogen-modified Pt–Fe alloy nanoparticles supported on ordered mesoporous carbons

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, Feng-Sheng [National Kaohsiung University of Applied Sciences, Department of Chemical and Materials Engineering (China); Liu, Shou-Heng, E-mail: shliu@mail.ncku.edu.tw [National Cheng Kung University, Department of Environmental Engineering (China); Kuo, Chung-Wen [National Kaohsiung University of Applied Sciences, Department of Chemical and Materials Engineering (China)

    2016-03-15

    A method has been demonstrated to synthesize nitrogen-modified Pt–Fe alloyed nanoparticles (9.2–11.3 nm) supported on ordered mesoporous carbon (Pt{sub x}Fe{sub 100−x}N/OMC), which is fabricated by a conventional wet chemical synthesis of Pt–Fe alloyed nanoparticles and followed by carbonization of the nanoparticles with tetraethylenepentamine as nitrogen chelating agent. Among these electrocatalysts, the Pt{sub 30}Fe{sub 70}N/OMC has highly catalytic activity for the oxygen reduction reaction (ORR) with significantly enhanced methanol tolerance as well. Combining the results from X-ray diffraction and X-ray absorption spectroscopy, it can be observed that Pt metal in the Pt{sub 30}Fe{sub 70}N/OMC is present in the outer shell of Pt–Fe alloys with face-centered cubic crystalline structure. By X-ray photoelectron spectroscopy, the nitrogen-modified Pt surface of Pt{sub 30}Fe{sub 70}N/OMC exhibits significant selectivity toward the ORR in the presence of methanol. This enhancement of methanol tolerance could be attributed to the inhibition of methanol adsorption resulting from the modification of the Pt surface with nitrogen.

  5. Synthesis, characterization, and electrochemical performance of nitrogen-modified Pt–Fe alloy nanoparticles supported on ordered mesoporous carbons

    International Nuclear Information System (INIS)

    Zheng, Feng-Sheng; Liu, Shou-Heng; Kuo, Chung-Wen

    2016-01-01

    A method has been demonstrated to synthesize nitrogen-modified Pt–Fe alloyed nanoparticles (9.2–11.3 nm) supported on ordered mesoporous carbon (Pt x Fe 100−x N/OMC), which is fabricated by a conventional wet chemical synthesis of Pt–Fe alloyed nanoparticles and followed by carbonization of the nanoparticles with tetraethylenepentamine as nitrogen chelating agent. Among these electrocatalysts, the Pt 30 Fe 70 N/OMC has highly catalytic activity for the oxygen reduction reaction (ORR) with significantly enhanced methanol tolerance as well. Combining the results from X-ray diffraction and X-ray absorption spectroscopy, it can be observed that Pt metal in the Pt 30 Fe 70 N/OMC is present in the outer shell of Pt–Fe alloys with face-centered cubic crystalline structure. By X-ray photoelectron spectroscopy, the nitrogen-modified Pt surface of Pt 30 Fe 70 N/OMC exhibits significant selectivity toward the ORR in the presence of methanol. This enhancement of methanol tolerance could be attributed to the inhibition of methanol adsorption resulting from the modification of the Pt surface with nitrogen.

  6. Controlled synthesis of mesoporous β-Ni(OH)2 and NiO nanospheres with enhanced electrochemical performance

    International Nuclear Information System (INIS)

    Xing, Shengtao; Wang, Qian; Ma, Zichuan; Wu, Yinsu; Gao, Yuanzhe

    2012-01-01

    Highlights: ► Uniform mesoporous β-Ni(OH) 2 and NiO nanospheres with hierarchical structures were synthesized by a simple complexation–precipitation method. ► Both ammonia and citrate played an important role for the formation of mesoporous nanospheres. ► β-Ni(OH) 2 and NiO nanospheres showed excellent capacitive properties due to their mesoporous structures and larger surface areas. -- Abstract: Uniform mesoporous β-Ni(OH) 2 and NiO nanospheres with hierarchical structures were synthesized by a facile complexation–precipitation method. The effects of ammonia and citrate on the structure and morphology of the products were thoroughly investigated by X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy and nitrogen adsorption–desorption measurements. The results indicated that ammonia played an important role for the formation of flowerlike spheres assembled from nanosheets. The addition of citrate could remarkably reduce the particle sizes and increase the specific surface areas of flowerlike spheres. A possible formation mechanism based on the experimental results was proposed to understand their growing procedures. β-Ni(OH) 2 and NiO nanospheres prepared with the addition of citrate showed excellent capacitive properties due to their mesoporous structures and large surface areas, suggesting the importance of controlled synthesis of hierarchical nanostructures for their applications.

  7. Nickel oxide/polypyrrole/silver nanocomposites with core/shell/shell structure: Synthesis, characterization and their electrochemical behaviour with antimicrobial activities

    Energy Technology Data Exchange (ETDEWEB)

    Das, Dhaneswar; Nath, Bikash C. [Department of Chemical Sciences, Tezpur University, Tezpur 784028, Assam (India); Phukon, Pinkee [Department of Molecular Biology and Biotechnology, Tezpur University, Tezpur 784028, Assam (India); Saikia, Bhaskar J.; Kamrupi, Isha R. [Department of Chemical Sciences, Tezpur University, Tezpur 784028, Assam (India); Dolui, Swapan K., E-mail: dolui@tezu.ernet.in [Department of Chemical Sciences, Tezpur University, Tezpur 784028, Assam (India)

    2013-10-01

    Magnetic and conducting Nickel oxide–polypyrrole (NiO/PPy) nanoparticles with core–shell structure were prepared in the presence of Nickel oxide (NiO) in aqueous solution containing sodium dodecyl benzenesulfonate (SDBS) as a surfactant as well as dopant. A stable dispersion of silver (Ag) nanoparticles was synthesized by chemical (citrate reduction) method. NiO/PPy nanocomposites were added to the Ag colloid under stirring. Ag nanoparticles could be electrostatically attracted on the surface of NiO/PPy nanocomposites, leading to formation of NiO/PPy/Ag nanocomposites with core/shell/shell structure. The morphology, structure, particle size and composition of the products were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, cyclic voltammetry (CV) and current–voltage (I–V) analysis. The resultant nanocomposites have the good conductivity and excellent electrochemical and catalytic properties of PPy and Ag nanoparticles. Furthermore, the nanocomposites showed excellent antibacterial behaviour due to the presence of Ag nanoparticles in the composite. The thermal stability of NiO–PPy as well as NiO/PPy/Ag nanocomposites was higher than that of pristine PPy. Studies of IR spectra suggest that the increased thermal stability may be due to interactions between NiO and Ag nanoparticles with the PPy backbone. - Highlights: • NiO nanoparticles were synthesized by two step soft chemical synthesis route. • Ag nanoparticles were prepared by using citrate reduction method. • NiO/PPy nanocomposites are synthesized by chemical oxidative polymerization process. • NiO/PPy/Ag nanocomposites can be used in the water purification technology.

  8. Nickel oxide/polypyrrole/silver nanocomposites with core/shell/shell structure: Synthesis, characterization and their electrochemical behaviour with antimicrobial activities

    International Nuclear Information System (INIS)

    Das, Dhaneswar; Nath, Bikash C.; Phukon, Pinkee; Saikia, Bhaskar J.; Kamrupi, Isha R.; Dolui, Swapan K.

    2013-01-01

    Magnetic and conducting Nickel oxide–polypyrrole (NiO/PPy) nanoparticles with core–shell structure were prepared in the presence of Nickel oxide (NiO) in aqueous solution containing sodium dodecyl benzenesulfonate (SDBS) as a surfactant as well as dopant. A stable dispersion of silver (Ag) nanoparticles was synthesized by chemical (citrate reduction) method. NiO/PPy nanocomposites were added to the Ag colloid under stirring. Ag nanoparticles could be electrostatically attracted on the surface of NiO/PPy nanocomposites, leading to formation of NiO/PPy/Ag nanocomposites with core/shell/shell structure. The morphology, structure, particle size and composition of the products were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, cyclic voltammetry (CV) and current–voltage (I–V) analysis. The resultant nanocomposites have the good conductivity and excellent electrochemical and catalytic properties of PPy and Ag nanoparticles. Furthermore, the nanocomposites showed excellent antibacterial behaviour due to the presence of Ag nanoparticles in the composite. The thermal stability of NiO–PPy as well as NiO/PPy/Ag nanocomposites was higher than that of pristine PPy. Studies of IR spectra suggest that the increased thermal stability may be due to interactions between NiO and Ag nanoparticles with the PPy backbone. - Highlights: • NiO nanoparticles were synthesized by two step soft chemical synthesis route. • Ag nanoparticles were prepared by using citrate reduction method. • NiO/PPy nanocomposites are synthesized by chemical oxidative polymerization process. • NiO/PPy/Ag nanocomposites can be used in the water purification technology

  9. SYNTHESIS, STEREOCHEMISTRY AND ANTIMICROBIAL ...

    African Journals Online (AJOL)

    Preferred Customer

    KEY WORDS: 4-Phenylsemicarbazone, Metal complexes, Stereochemistry, Antimicrobial activity. INTRODUCTION ... stereochemistry of semicarbazone metal complexes [8-13], this group of ligands deserve further investigations. ..... The cytotoxicity of tested compounds generally increased with increase concentration and ...

  10. In situ synthesis, electrochemical and quantum chemical analysis of an amino acid-derived ionic liquid inhibitor for corrosion protection of mild steel in 1M HCl solution

    International Nuclear Information System (INIS)

    Kowsari, E.; Arman, S.Y.; Shahini, M.H.; Zandi, H.; Ehsani, A.; Naderi, R.; PourghasemiHanza, A.; Mehdipour, M.

    2016-01-01

    Highlights: • Electrochemical analysis of effectiveness of an amino acid-derived ionic liquid inhibitor. • Quantum chemical analysis of effectiveness of an amino acid-derived ionic liquid inhibitor. • Finding correlation between electrochemical analysis and quantum chemical analysis. - Abstract: In this study, an amino acid-derived ionic liquid inhibitor, namely tetra-n-butyl ammonium methioninate, was synthesized and the role this inhibitor for corrosion protection of mild steel exposed to 1.0 M HCl was investigated using electrochemical, quantum and surface analysis. By taking advantage of potentiodynamic polarization, the inhibitory action of tetra-n-butyl ammonium methioninate was found to be mainly mixed-type with dominant anodic inhibition. The effectiveness of the inhibitor was also indicated using electrochemical impedance spectroscopy (EIS). Moreover, to provide further insight into the mechanism of inhibition, electrochemical noise (EN) and quantum chemical calculations of the inhibitor were performed.

  11. Expanding the family of heteroleptic oxidovanadium(IV) compounds with salicylaldehyde semicarbazones and polypyridyl ligands showing anti-Trypanosoma cruzi activity.

    Science.gov (United States)

    Scalese, Gonzalo; Benítez, Julio; Rostán, Santiago; Correia, Isabel; Bradford, Lara; Vieites, Marisol; Minini, Lucía; Merlino, Alicia; Coitiño, E Laura; Birriel, Estefania; Varela, Javier; Cerecetto, Hugo; González, Mercedes; Pessoa, João Costa; Gambino, Dinorah

    2015-06-01

    Searching for prospective vanadium-based drugs for the treatment of Chagas disease, a new series of heteroleptic [V(IV)O(L-2H)(NN)] compounds was developed by including the lipophilic 3,4,7,8-tetramethyl-1,10-phenanthroline (tmp) NN ligand and seven tridentate salicylaldehyde semicarbazone derivatives (L1-L7). The compounds were characterized in the solid state and in solution. EPR spectroscopy suggests that the NN ligand is bidentate bound through both nitrogen donor atoms in an axial-equatorial mode. The EPR and (51)V-NMR spectra of aerated solutions at room temperature indicate that the compounds are stable to hydrolysis and that no significant oxidation of V(IV) to V(V) takes place at least in 24h. The complexes are more active in vitro against Trypanosoma cruzi, the parasite responsible for Chagas disease, than the reference drug Nifurtimox and most of them are more active than previously reported [V(IV)O(L-2H)(NN)] complexes of other NN co-ligands. Selectivity towards the parasite was analyzed using J-774 murine macrophages as mammalian cell model. Due to both, high activity and high selectivity, L2, L4, L5 and L7 complexes could be considered new hits for further drug development. Lipophilicity probably plays a relevant role in the bioactivity of the new compounds. The [V(IV)O(L-2H)(NN)] compounds were designed aiming DNA as potential molecular target. Therefore, the novel L1-L7 tmp complexes were screened by computational modeling, comparing their DNA-binding features with those of previously reported [V(IV)O(L-2H)(NN)] compounds with different NN co-ligands. Whereas all the complexes interact well with DNA, with binding modes and strength tuned in different extents by the NN and semicarbazone co-ligands, molecular docking suggests that the observed anti-T. cruzi activity cannot be explained upon DNA intercalation as the sole mechanism of action. Copyright © 2015 Elsevier Inc. All rights reserved.

  12. Synthesis, structure and electrochemical properties of LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F fluoride-phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Fedotov, Stanislav S. [Department of Chemistry, Lomonosov Moscow State University, 119991 Moscow (Russian Federation); Skoltech Center for Electrochemical Energy Storage, Skolkovo Institute of Science and Technology, 143026 Moscow (Russian Federation); Kuzovchikov, Sergey M.; Khasanova, Nellie R.; Drozhzhin, Oleg A.; Filimonov, Dmitriy S. [Department of Chemistry, Lomonosov Moscow State University, 119991 Moscow (Russian Federation); Karakulina, Olesia M.; Hadermann, Joke [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Abakumov, Artem M. [Department of Chemistry, Lomonosov Moscow State University, 119991 Moscow (Russian Federation); Skoltech Center for Electrochemical Energy Storage, Skolkovo Institute of Science and Technology, 143026 Moscow (Russian Federation); EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Antipov, Evgeny V. [Department of Chemistry, Lomonosov Moscow State University, 119991 Moscow (Russian Federation)

    2016-10-15

    LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F fluoride-phosphate was synthesized via conventional solid-state and novel freeze-drying routes. The crystal structure was refined based on neutron powder diffraction (NPD) data and validated by electron diffraction (ED) and high-resolution transmission electron microscopy (HRTEM). The alkali ions are ordered in LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F and the transition metals jointly occupy the same crystallographic sites. The oxidation state and oxygen coordination environment of the Fe atoms were verified by {sup 57}Fe Mössbauer spectroscopy. Electrochemical tests of the LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F cathode material demonstrated a reversible activity of the Fe{sup 3+}/Fe{sup 2+} redox couple at the electrode potential near 3.4 V and minor activity of the Co{sup 3+}/Co{sup 2+} redox couple over 5 V vs Li/Li{sup +}. The material exhibited the discharge capacity of more than 82% (theo.) regarding Fe{sup 3+}/Fe{sup 2+} in the 2.4÷4.6 V vs Li/Li{sup +} potential range. - Graphical abstract: The ball-polyhedral representation of the LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F crystal structure. The MO{sub 4}F{sub 2} units are depicted as blue octahedra, PO{sub 4} units as orange tetrahedra, sodium atoms are designated as yellow (Na1), lithium – red and brown (Li2, Li3 resp.), fluorine – green, oxygen – violet spheres. - Highlights: • Freeze-drying method was successfully applied to the synthesis of LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F. • The crystal structure of LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F was refined based on NPD and validated by ED and HRTEM. • LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F demonstrated a reversible Li de/intercalation in the 2.5÷4.6 V vs Li/Li{sup +} range.

  13. 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

    2015-01-01

    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. PMID:26577799

  14. Aerosol synthesis and electrochemical analysis of niobium mixed-metal oxides for the ethanol oxidation reaction in acid and alkaline electrolyte

    Science.gov (United States)

    Konopka, Daniel A.

    Direct ethanol fuel cells are especially important among emerging electrochemical power systems with the potential to offset a great deal of the energy demand currently met through the use of fossil fuels. Ethanol can be refined from petroleum sources or attained from renewable biomass, and is more easily and safely stored and transported than hydrogen, methanol or gasoline. The full energy potential of ethanol in fuel cells can only be realized if the reaction follows a total oxidation pathway to produce CO2. This must be achieved by the development of advanced catalysts that are electrically conductive, stable in corrosive environments, contain a high surface area on which the reaction can occur, and exhibit a bi-functional effect for the ethanol oxidation reaction (EOR). The latter criterion is achievable in mixed-metal systems. Platinum is an effective metal for catalyzing surface reactions of many adsorbates and is usually implemented in the form of Pt nanoparticles supported on inexpensive carbon. This carbon is believed to be neutral in the catalysis of Pt. Instead, carbon can be replaced with carefully designed metals and metal oxides as co-catalysis or support structures that favorably alter the electronic structure of Pt slightly through a strong metal support interaction, while also acting as an oxygen source near adsorbates to facilitate the total oxidation pathway. Niobium mixed-metal-oxides were explored in this study as bi-functional catalyst supports to Pt nanoparticles. We developed a thermal aerosol synthesis process by which mesoporous powders of mixed-metal-oxides decorated with Pt nanoparticles could be obtained from liquid precursors within ˜5 seconds or less, followed by carefully refined chemical and thermal post-treatments. Exceptionally high surface areas of 170--180m2/g were achieved via a surfactant-templated 3D wormhole-type porosity, comparable on a per volume basis to commercial carbon blacks and high surface area silica supports

  15. Electrochemical Cell

    DEFF Research Database (Denmark)

    1999-01-01

    The invention relates to a rechargeable electrochemical cell comprising a negative electrode, an electrolyte and a positive electrode in which the positive electrode structure comprises a lithium cobalt manganese oxide of the composition Li¿2?Co¿y?Mn¿2-y?O¿4? where 0 ... for capacity losses in lithium ion cells and lithium-alloy cells....

  16. Electrochemical capacitor

    Science.gov (United States)

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

    1999-10-05

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

  17. synthesis, optical and electrochemical characterization

    African Journals Online (AJOL)

    a

    a working electrode, a silver wire quasi reference electrode directly placed into the electrolyte solution and a platinum wire as counter electrode were used. The polymer ... The cathodes were made by evaporating LiF (0.5 nm)/Al (60 nm) in vacuum ∼. 10-6 Torr. The diodes were defined by a mask with an active area of 4 ...

  18. ELECTROCHEMICAL SYNTHESIS AND CHARACTERIZATION OF ...

    African Journals Online (AJOL)

    examples of materials used in redox capacitor electrodes. Several studies proved that making a hybrid material of conjugated polymers with transition metal oxides [5-8], carbon nanomaterials [5-8], polyoxometalates [9-12], and quinone containing biomaterials [12-16] significantly improve the energy storage capacity of SCs ...

  19. Synthesis, photophysical, electrochemical and electroluminescence ...

    Indian Academy of Sciences (India)

    FARMAN ALI

    2017-09-04

    Sep 4, 2017 ... N)2Ir(acac) complexes in toluene showed phosphorescence (λmax = 598 nm to 658 nm) with quantum yields (0.1 to 0.32) and microsecond lifetimes (0.43 to 1.9 μs). The complexes were non-luminescent in thin films due to self-quenching but luminescent when lightly doped (5%) in a host organic material, ...

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

    Science.gov (United States)

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

    2016-06-01

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

  1. Influence of ionic liquid on pseudocapacitance performance of electrochemically synthesized conductive polymer: Electrochemical and theoretical investigation.

    Science.gov (United States)

    Ehsani, A; Kowsari, E; Dashti Najafi, M; Safari, R; Mohammad Shiri, H

    2017-08-15

    This study demonstrates a method for improving supercapacitive performance of electrochemically synthesized conductive polymer. In this regards, 1-Butyl-3-methyl imidazolium hexafluorophosphate (BI) as a new high efficient ionic liquid was synthesized using chemical approach and then fabricated POAP/BI films by electro-polymerization of POAP in the presence of BI to serve as the active electrode for electrochemical supercapacitor. Theoretical study (AIM) and electrochemical analysis have been used for characterization of ionic liquid and POAP/BI composite film. Different electrochemical methods including galvanostatic charge-discharge experiments, cyclic voltammetry and electrochemical impedance spectroscopy are carried out in order to investigate the performance of the system. This work introduces new most efficient materials for electrochemical redox capacitors with advantages including ease synthesis, high active surface area and stability in an aqueous electrolyte. Copyright © 2017 Elsevier Inc. All rights reserved.

  2. Electrochemical cell

    Science.gov (United States)

    Redey, L.I.; Myles, K.M.; Vissers, D.R.; Prakash, J.

    1996-07-02

    An electrochemical cell is described with a positive electrode having an electrochemically active layer of at least one transition metal chloride. A negative electrode of an alkali metal and a compatible electrolyte including an alkali metal salt molten at cell operating temperature is included in the cell. The electrolyte is present at least partially as a corrugated {beta}{double_prime} alumina tube surrounding the negative electrode interior to the positive electrode. The ratio of the volume of liquid electrolyte to the volume of the positive electrode is in the range of from about 0.1 to about 3. A plurality of stacked electrochemical cells is disclosed each having a positive electrode, a negative electrode of an alkali metal molten at cell operating temperature, and a compatible electrolyte. The electrolyte is at least partially present as a corrugated {beta}{double_prime} alumina sheet separating the negative electrode and interior to the positive electrodes. The alkali metal is retained in a porous electrically conductive ceramic, and seals for sealing the junctures of the electrolyte and the adjacent electrodes at the peripheries thereof. 8 figs.

  3. 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.

  4. SHORT COMMUNICATION SYNTHESIS AND PRELIMINARY ...

    African Journals Online (AJOL)

    a

    amino]antipyrine semicarbazone. INTRODUCTION. Thiosemicarbazones and their metal complexes have been the subject of extensive investigations because of their potential pharmacological properties and a wide variation in their modes of.

  5. AlOOH-reduced graphene oxide nanocomposites: one-pot hydrothermal synthesis and their enhanced electrochemical activity for heavy metal ions.

    Science.gov (United States)

    Gao, Chao; Yu, Xin-Yao; Xu, Ren-Xia; Liu, Jin-Huai; Huang, Xing-Jiu

    2012-09-26

    This work described the preparation, characterization, and electrochemical behavior toward heavy metal ions of the AlOOH-reduced graphene oxide nanocomposites. This new material was synthesized through a green one-pot hydrothermal method. The morphologic and structure of the nanocomposites were characterized using atomic force microscopy, X-ray diffraction, Raman spectroscopy, X-ray photoemission spectroscopy, Fourier transform-infrared spectroscopy, and transmission electron microscopy. Electrochemical properties were characterized by cyclic voltammetry and electrochemical impedance spectroscopy. The chemical and electrochemical parameters that have influence on deposition and stripping of metal ions, such as pH value, deposition potential, and deposition time, were also studied. Due to the strong affinity of AlOOH to heavy metal ions and the fast electron-transfer kinetics of graphene, the combination of solid-phase extraction and stripping voltammetric analysis allowed fast and sensitive determination of Cd(II) and Pb(II) in drinking water, making these new nanocomposites promising candidates for practical applications in the fields of detecting heavy metal ions. Most importantly, these new nanocomposites may possess many unknown properties waiting to be explored.

  6. Synthesis, photophysics, structure-tunable photoluminescence, and electrochemical properties of soluble poly(p-phenylenevinylene)-based polymers with adjacent 1,3,4-oxadiazoles in the backbone

    Czech Academy of Sciences Publication Activity Database

    Mikroyannidis, J. A.; Hlídková, Helena; Výprachtický, Drahomír; Cimrová, Věra

    2005-01-01

    Roč. 43, č. 14 (2005), s. 3079-3090 ISSN 0887-624X R&D Projects: GA AV ČR IAA4050409 Institutional research plan: CEZ:AV0Z40500505 Keywords : electrochemical properties * Heck coupling * light emitting polymers Subject RIV: CD - Macromolecular Chemistry Impact factor: 3.027, year: 2005

  7. Facile one-pot synthesis of spherical zinc sulfide-carbon nanocomposite powders with superior electrochemical properties as anode materials for Li-ion batteries.

    Science.gov (United States)

    Jang, Yong Seung; Kang, Yun Chan

    2013-10-21

    A novel and simple one-pot method of systematically synthesizing spherical metal sulfide-carbon composite powders is reported for the first time. The zinc sulfide-carbon composite is selected as the first target material. The prepared composite powders show superior electrochemical properties as anode materials for lithium-ion batteries.

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

    Science.gov (United States)

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

    2017-10-19

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

  9. 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 Ti0.7W0.3O2 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. Ti0.7W0.3O2 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 Ti0.7W0.3O2 are comparable to those of commercial Pt on carbon black.

  10. Electrochemical cell

    Science.gov (United States)

    Kaun, T.D.

    An improved secondary electrochemical cell is disclosed having a negative electrode of lithium aluminum, a positive electrode of iron sulfide, a molten electrolyte of lithium chloride and potassium chloride, and the combination that the fully charged theoretical capacity of the negative electrode is in the range of 0.5 to 1.0 that of the positive electrode. The cell thus is negative electrode limiting during discharge cycling. Preferably, the negative electrode contains therein, in the approximate range of 1 to 10 volume % of the electrode, an additive from the materials of graphitized carbon, aluminum-iron alloy, and/or magnesium oxide.

  11. Synthesis of nano-particles by soft chemistry: structural, morphological and dimensional control. Studies of the electrochemical properties (towards dyes solar cells)

    International Nuclear Information System (INIS)

    Cassaignon, S.; Koelsch, M.; Jolivet, J.P.

    2006-01-01

    In this work are described the electrochemical behaviour of different TiO 2 films (anatase, brookite and rutile) in aqueous solution and the influence of the parameters as the crystal structure and the morphology on the electrochemical answer. To complete this study, the capacity of the double layer has been measured by impedance spectroscopy. Voltage measurements of TiO 2 sensitized by a dye will allow to discuss the reversibility of the system and the rearrangement mechanisms. At last, the influence of the nature of the TiO 2 particles (anatase, rutile and brookite) on the photovoltage has been studied in order to estimate their interest for photovoltaic devices. (O.M.)

  12. The Synthesis of Novel 3-Substituted Poly(pyrroles) Bearing Crown-ether Moieties and a Study of their Electrochemical Properties

    DEFF Research Database (Denmark)

    Guernion, Nicolas J.L.; Blencowe, A.; Hayes, Wayne

    2006-01-01

    and galvanostatic modes and the electrochemical properties of those systems were studied via cycling voltammetry in aqueous and organic media. Novel crown-ether substituted polypyrrole derivatives revealed reversible redox couples in LiClO4/CH3CN (0.1 M). The morphology of these novel crown-ether substituted...... polypyrrole derivatives was characterised by Scanning Electron Microscopy (SEM). These polymers exhibited an open porous structure and half the charge was required when compared to polypyrrole to afford films of equal thickness. The mass change during polymerisation was followed by Electrochemical Quartz...... Crystal Microbalance measurement (EQCM), and the rate of polymer growth was found to be non-linear when compared to polypyrrole....

  13. The electrochemical synthesis and corrosion behaviour of TiO2/poly(indole-co-aniline multilayer coating: Experimental and theoretical approach

    Directory of Open Access Journals (Sweden)

    Serap Toprak Döşlü

    2018-01-01

    Full Text Available The aim of this study was to protect stainless steel against corrosion via poly (indole-co-aniline with the help of titanium dioxide pre-coating. Different monomer ratios (1:1 and 1:9 were applied in order to determine the suitable chain composition to synthesize the copolymer in lithium perchlorate containing acetonitrile. The structures, morphologies, electrochemical properties and corrosion resistances of the mono and multi-layer coatings were investigated by Fourier-transform infrared spectra, scanning electron microscope, energy dispersive X-ray spectrometer, electrochemical impedance spectroscopy and anodic polarization. Furthermore the geometric structure and electronic properties of indole, aniline, and indole-co-aniline (dimmer molecules have been investigated by quantum calculations. The results indicated that corrosion protection of copolymers was increased via titanium dioxide pre-coating. The 1:1 copolymer coating showed better corrosion prevention than 1:9 coating. The correlation was determined between experimental and theoretical parameters.

  14. Electrochemical Co-Reduction Synthesis of AuPt Bimetallic Nanoparticles-Graphene Nanocomposites for Selective Detection of Dopamine in the Presence of Ascorbic Acid and Uric Acid

    Directory of Open Access Journals (Sweden)

    Zongya Zhao

    2015-07-01

    Full Text Available In this paper, AuPt bimetallic nanoparticles-graphene nanocomposites were obtained by electrochemical co-reduction of graphene oxide (GO, HAuCl4 and H2PtCl6. The as-prepared AuPt bimetallic nanoparticles-graphene nanocomposites were characterized by scanning electron microscopy (SEM, electrochemical impedance spectroscopy (EIS and other electrochemical methods. The morphology and composition of the nanocomposite could be easily controlled by adjusting the HAuCl4/H2PtCl6 concentration ratio. The electrochemical experiments showed that when the concentration ratio of HAuCl4/H2PtCl6 was 1:1, the obtained AuPt bimetallic nanoparticles-graphene nanocomposite (denoted as Au1Pt1NPs-GR possessed the highest electrocatalytic activity toward dopamine (DA. As such, Au1Pt1NPs-GR nanocomposites were used to detect DA in the presence of ascorbic acid (AA and uric acid (UA using the differential pulse voltammetry (DPV technique and on the modified electrode, there were three separate DPV oxidation peaks with the peak potential separations of 177 mV, 130 mV and 307 mV for DA and AA, DA and UA, AA and UA, respectively. The linear range of the constructed DA sensor was from 1.6 μM to 39.7 μM with a detection limit of 0.1 μM (S/N = 3. The obtained DA sensor with good stability, high reproducibility and excellent selectivity made it possible to detect DA in human urine samples.

  15. Single step synthesis of gold-amino acid composite, with the evidence of the catalytic hydrogen atom transfer (HAT) reaction, for the electrochemical recognition of Serotonin

    Science.gov (United States)

    Choudhary, Meenakshi; Siwal, Samarjeet; Nandi, Debkumar; Mallick, Kaushik

    2016-03-01

    A composite architecture of amino acid and gold nanoparticles has been synthesized using a generic route of 'in-situ polymerization and composite formation (IPCF)' [1,2]. The formation mechanism of the composite has been supported by a model hydrogen atom (H•≡H++e-) transfer (HAT) type of reaction which belongs to the proton coupled electron transfer (PCET) mechanism. The 'gold-amino acid composite' was used as a catalyst for the electrochemical recognition of Serotonin.

  16. A simple and efficient electrochemical reductive method for ...

    Indian Academy of Sciences (India)

    The electrochemical reduction of graphene oxide typically involves complicated procedures, such as modification of electrodes and preparation of electrolytes, which is often needed in previous reports. In this paper, a simple and efficient electrochemical process is described for the synthesis of high-quality reduced ...

  17. Synthesis, characterization and electrochemical performance of graphene decorated with 1D NiMoO4 · nH2O nanorods.

    Science.gov (United States)

    Ghosh, Debasis; Giri, Soumen; Das, Chapal Kumar

    2013-11-07

    One-dimensional NiMoO4 · nH2O nanorods and their graphene based hybrid composite with good electrochemical properties have been synthesized by a cost effective hydrothermal procedure. The formation of the mixed metal oxide and the composite was confirmed by XRD, XPS and Raman analyses. The morphological characterizations were carried out using FESEM and TEM analyses. The materials were subjected to electrochemical characterization through cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS) studies with 6 M KOH as the supporting electrolyte. For NiMoO4 · nH2O, a maximum specific capacitance of 161 F g(-1) was obtained at 5 A g(-1) current density, accompanied with an energy density of 4.53 W h kg(-1) at a steady power delivery rate of 1125 W kg(-1). The high utility of the pseudocapacitive NiMoO4 · nH2O was achieved in its graphene based composite, which exhibited a high specific capacitance of 367 F g(-1) at 5 A g(-1) current density and a high energy density of 10.32 W h kg(-1) at a power density of 1125 W kg(-1) accompanied with long term cyclic stability.

  18. High performance electrochemical pseudocapacitors from ionic liquid assisted electrochemically synthesized p-type conductive polymer.

    Science.gov (United States)

    Ehsani, A; Mohammad Shiri, H; Kowsari, E; Safari, R; Torabian, J; Hajghani, S

    2017-03-15

    In this paper firstly, 1-methyl-3-methylimidazolium bromide (MB) as a new high efficient ionic liquid was synthesized using chemical approach and then fabricated POAP/MB films by electro-polymerization of POAP in the presence of MB to serve as the active electrode for electrochemical supercapacitor. Theoretical study (AIM) and electrochemical analysis have been used for characterization of ionic liquid and POAP/MB composite film. Different electrochemical methods including galvanostatic charge-discharge experiments, cyclic voltammetry and electrochemical impedance spectroscopy are carried out in order to investigate the performance of the system. This work introduces new most efficient materials for electrochemical redox capacitors with advantages including ease synthesis, high active surface area and stability in an aqueous electrolyte. Copyright © 2016 Elsevier Inc. All rights reserved.

  19. Facile synthesis of the necklace-like graphene oxide-multi-walled carbon nanotube nanohybrid and its application in electrochemical sensing of Azithromycin

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Kaixin [Jiangxi Key Laboratory of Organic Chemistry, Jiangxi Science and Technology Normal University, Nanchang 330013 (China); Lu, Limin; Wen, Yangping [Jiangxi Key Laboratory of Organic Chemistry, Jiangxi Science and Technology Normal University, Nanchang 330013 (China); College of Science, Jiangxi Agricultural University, Nanchang 330045 (China); Xu, Jingkun, E-mail: xujingkun@tsinghua.org.cn [Jiangxi Key Laboratory of Organic Chemistry, Jiangxi Science and Technology Normal University, Nanchang 330013 (China); Duan, Xuemin; Zhang, Long; Hu, Dufen [Jiangxi Key Laboratory of Organic Chemistry, Jiangxi Science and Technology Normal University, Nanchang 330013 (China); Nie, Tao [Jiangxi Key Laboratory of Organic Chemistry, Jiangxi Science and Technology Normal University, Nanchang 330013 (China); College of Science, Jiangxi Agricultural University, Nanchang 330045 (China)

    2013-07-17

    Graphical abstract: -- Highlights: •The necklace-like GO-MWCNTs nanohybrid was facilely synthesized by ultrasonication. •The nanocomposites can be effectively used for the detection of Azithromycin. •Low detection limit with wide linear range could be obtained. •The method was applied to determine Azi in real samples. -- Abstract: A novel electrochemical platform was designed for the determination of Azithromycin (Azi), a widely used macrolide antibiotic, by combining the hydrophilic properties of graphene oxide (GO) and the excellent electronic and antifouling properties of multi-walled carbon nanotubes (MWCNTs). Stable MWCNTs aqueous dispersion has been prepared using GO nano-sheets as surfactant and the obtained GO-MWCNTs nanohybrid was characterized by UV–vis spectroscopy, Fourier transform infrared spectroscopy, Raman spectroscopy, transmission electron microscopy and electrochemical impedance spectroscopy, which confirmed that GO nano-sheets were attached onto the wall of MWCNTs to form a necklace-like structure. Electrochemical results obviously reveal that the oxidation peak currents of Azi obtained at the GC electrode modified with GO-MWCNTs hybrid are much higher than those at the MWCNTs/GC, GO/GC and bare GC electrodes. Under optimized conditions, the anodic peak current was linear to the concentration of Azi in the range from 0.1 to 10 μM with the detection limit of 0.07 μM. To further validate its possible application, the proposed method was successfully used for the determination of Azi in pharmaceutical formulations with satisfactory results.

  20. Synthesis of One Dimensional Li2MoO4 Nanostructures and Their Electrochemical Performance as Anode Materials for Lithium-ion Batteries

    International Nuclear Information System (INIS)

    Liu, Xudong; Zhao, Yanming; Dong, Youzhong; Fan, Qinghua; Kuang, Quan; Liang, Zhiyong; Lin, Xinghao; Han, Wei; Li, Qidong; Wen, Mingming

    2015-01-01

    Highlights: • One dimensional Li 2 MoO 4 nanostructures including nanorods and nanotubes have been successfully fabricated via a simple sol-gel method firstly. • Possible crystal formation mechanisms are proposed for these one dimensional Li 2 MoO 4 nanostructures. • These one dimensional Li 2 MoO 4 nanostructure electrode materials present outstanding rate abilities and cycle capabilities in electrochemical performance compared to the carbon-free powder sample when evaluated as anode materials for Lithium-ion batteries. • The carbon-coated Li 2 MoO 4 nanotube electrode improves the charging/discharging capacities of graphite even after applying 60 cycles at very high current density. - Abstract: One dimensional Li 2 MoO 4 nanostructures including nanorods and nanotubes have been successfully fabricated via a simple sol-gel method adding Li 2 CO 3 and MoO 3 powders into distilled water with citric acid as an assistant agent and carbon source. Our experimental results show that the formation of the one dimensional nanostructure morphology is evaporation and crystallization process with self-adjusting into a rod-like hexagonal cross-section structure, while the citric acid played an important role during the formation of Li 2 MoO 4 nanotubes under the acidic environment by capping, stabilizing the {1010} facet of Li 2 MoO 4 structure and controlling the concentration of H + (pH value) of the aqueous solution. Finally, basic electrochemical performance of these one dimensional Li 2 MoO 4 nanostructures including nanorods and nanotubes evaluated as anode materials for lithium-ion batteries (LIBs) are discussed, for comparison, the properties of carbon-free powder sample synthesized by solid-state reaction are also displayed. Experimental results show that different morphology and carbon-coating on the surface have an important influence on electrochemical performance

  1. In situ electrochemical synthesis of highly loaded zirconium nanoparticles decorated reduced graphene oxide for the selective determination of dopamine and paracetamol in presence of ascorbic acid.

    Science.gov (United States)

    Ezhil Vilian, A T; Rajkumar, Muniyandi; Chen, Shen-Ming

    2014-03-01

    Highly loaded zirconium oxide (ZrO2) nanoparticles were supported on graphene oxide (ERGO/ZrO2) via an in situ, simple and clean strategy on the basis of the electrochemical redox reaction between zirconyl chloride and graphene oxide (ZrOCl2 and GO). The electrochemical measurements and surface morphology of the as prepared nanocomposite were studied using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and field emission scanning electron microscopy (FESEM). This ZrO2 decorated reduced graphene oxide nanocomposite modified GCE (ERGO/ZrO2) exhibits a prominent electrocatalytic activity toward the selective detection and determination of dopamine (DA) and paracetamol (PA) in presence of ascorbic acid (AA). The peaks of linear sweep voltammetry (LSV) for DA and PA oxidation at ERGO/ZrO2 modified electrode surface were clearly separated from each other when they co-existed in the physiological pH (pH 7.0) with a potential value of 140 mV (between AA and DA) and 330 mV (between AA and PA). It was, therefore, possible to simultaneously determine DA and PA in the samples at ERGO/ZrO2 nanocomposite modified GCE. Linear calibration curves were obtained for 9-237 μM of PA and DA. The ERGO/ZrO2 nanocomposite electrode has been satisfactorily used for the determination of DA and PA in the presence of AA at pharmaceutical formulations in human urine samples with a linear range of 3-174 μM. The proposed biosensor shows a wide linear range, low detection limit, good reproducibility and acceptable stability, providing a biocompatible platform for bio sensing and bio catalysis. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. 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

  3. Nanoscale Electrochemical Sensing and Processing in Microreactors.

    Science.gov (United States)

    Odijk, Mathieu; van den Berg, Albert

    2018-03-08

    In this review, we summarize recent advances in nanoscale electrochemistry, including the use of nanoparticles, carbon nanomaterials, and nanowires. Exciting developments are reported for nanoscale redox cycling devices, which can chemically amplify signal readout. We also discuss promising high-frequency techniques such as nanocapacitive CMOS sensor arrays or heterodyning. In addition, we review electrochemical microreactors for use in (drug) synthesis, biocatalysis, water treatment, or to electrochemically degrade urea for use in a portable artificial kidney. Electrochemical microreactors are also used in combination with mass spectrometry, e.g., to study the mimicry of drug metabolism or to allow electrochemical protein digestion. The review concludes with an outlook on future perspectives in both nanoscale electrochemical sensing and electrochemical microreactors. For sensors, we see a future in wearables and the Internet of things. In microreactors, a future goal is to monitor the electrochemical conversions more precisely or ultimately in situ by combining other spectroscopic techniques. Expected final online publication date for the Annual Review of Analytical Chemistry Volume 11 is June 12, 2018. Please see http://www.annualreviews.org/page/journal/pubdates for revised estimates.

  4. Impacts of synthesis temperature and carbon content on the electrochemical performances of the Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C composite synthesized by a polyol method

    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, 710055 Xi' an (China); Zhang, Haipeng; Zheng, Siqi [Shaanxi Key Laboratory of Nanomaterials and Nanotechnology, Xi' an University of Architecture and Technology, 710055 Xi' an (China); Hojamberdiev, Mirabbos [Materials and Structures Laboratory, Tokyo Institute of Technology, 4259 Nagatsuta, Midori, Yokohama, Kanagawa 226-8503 (Japan); Ren, Bing; Xu, Yunhua; Shao, Chongyang [Shaanxi Key Laboratory of Nanomaterials and Nanotechnology, Xi' an University of Architecture and Technology, 710055 Xi' an (China)

    2014-12-15

    As a cathode material for Li-ion battery, Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} was synthesized by a polyol method using LiOH·H{sub 2}O, V{sub 2}O{sub 5}, NH{sub 4}H{sub 2}PO{sub 4}, sucrose, and ethylene glycol as starting materials. Under the polyol process, the impacts of synthesis parameters, including the sintering temperature, holding time, and carbon content, on the morphological evolution and electrochemical properties of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} were investigated. The XRD results show the formation of pure Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} with monoclinic crystal structure. The images of SEM show the similar-spherical morphology with uniform and optimized particles size, which greatly improves the electrochemical performance. The carbon coated on the Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} particles was clearly observed by electron microscopy. The particle size of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} powders gradually decreases with the increase of carbon content in composite. In the potential range of 3.0–4.3 V, the composite synthesized at 800 °C for 10 h with 10% carbon content shows the highest discharge capacity of 128 mAh g{sup −1} at 0.1C, which is nearly close to the theoretical capacity, and it remains fairly stable (more than 126 mAh g{sup −1}) even after the 20th cycles. Based on the results from the electrochemical impedance spectroscopy (EIS) analysis, the apparent diffusion coefficients of Li ions in the composite materials are between 1.82 × 10{sup −10} and 3.79 × 10{sup −9} cm{sup 2} s{sup −1}, which are much higher than those of olivine LiFePO{sub 4}. - Highlights: • As a cathode material, Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C was successfully synthesized by polyol method. • Impacts of synthesis temperature, holding time and carbon content were studied. • Electrochemical performance of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} was affected by particle morphology and size. • Li{sub 3}V{sub 2}(PO{sub 4

  5. Synthesis and Electrochemical Performance of Graphene Wrapped SnxTi1−xO2 Nanoparticles as an Anode Material for Li-Ion Batteries

    Directory of Open Access Journals (Sweden)

    Xing Xin

    2015-01-01

    Full Text Available Ever-growing development of Li-ion battery has urged the exploitation of new materials as electrodes. Here, SnxTi1-xO2 solid-solution nanomaterials were prepared by aqueous solution method. The morphology, structures, and electrochemical performance of SnxTi1-xO2 nanoparticles were systematically investigated. The results indicate that Ti atom can replace the Sn atom to enter the lattice of SnO2 to form substitutional solid-solution compounds. The capacity of the solid solution decreases while the stability is improved with the increasing of the Ti content. Solid solution with x of 0.7 exhibits the optimal electrochemical performance. The Sn0.7Ti0.3O2 was further modified by highly conductive graphene to enhance its relatively low electrical conductivity. The Sn0.7Ti0.3O2/graphene composite exhibits much improved rate performance, indicating that the SnxTi1-xO2 solid solution can be used as a potential anode material for Li-ion batteries.

  6. Synthesis, Photophysical and Electrochemical Properties of a Mixed Bipyridyl-Phenanthrolyl Ligand Ru(II Heteroleptic Complex Having trans-2-Methyl-2-butenoic Acid Functionalities

    Directory of Open Access Journals (Sweden)

    Adewale O. Adeloye

    2011-09-01

    Full Text Available In this work, two ligands: 4-(trans-2-Methyl-2-butenoic acid-2,2'-bipyridine (L1 and 5-(trans-2-methyl-2-butenoic acid-1,10-phenanthroline (L2, with the corresponding mixed-ligand heteroleptic Ru(II complex were synthesized and characterized by FT-IR, 1H-, 13C-NMR spectroscopy and elemental analysis. The influence of the mixed functionalized polypyridyl ruthenium(II complex on the photophysical and electrochemical properties were investigated and compared to individual single-ligand homoleptic complexes. Interestingly, the mixed-ligand complex formulated as [RuL1L2(NCS2] exhibits broad and intense metal-to-ligand charge transfer (MLCT absorption with a high molar extinction coefficient (λmax = 514 nm, ε = 69,700 M−1 cm−1, better than those of individual single-ligand complexes, [Ru(L12(NCS2] and [Ru(L22(NCS2], and a strong photoluminescence intensity ratio in the red region at λem = 686 nm. The electrochemical properties of the complex indicated that the redox processes are ligand-based.

  7. Hydrothermal synthesis of red phosphorus @reduced graphene oxide nanohybrid with enhanced electrochemical performance as anode material of lithium-ion battery

    Science.gov (United States)

    Zhu, Xing; Yuan, Zewei; Wang, Xiaobo; Jiang, Guodong; Xiong, Jian; Yuan, Songdong

    2018-03-01

    Red phosphorus @reduced graphene oxide (P @rGO) nanohybrid was synthesized via a two-step hydrothermal process. The obtained P @rGO nanohybrid was characterized by TEM, SEM, Raman, XRD and XPS. It was found that the nano-scale red phosphorus encapsulated in the reduced graphene oxide and the existence of phosphorus promote the reduction of graphene oxide. The electrochemical performance of P @rGO nanohybrid as an anode material was investigated by galvanostatic charge/discharge, rate performance, cyclic voltammetry and AC impedance test. With increasing the mass of rGO, the electrochemical performance of P @rGO nanohybrid was significantly enhanced. The first discharge/charge specific capacity of the nanohybrid prepared at optimum condition (P:GO = 7:3) could achieve approximately 2400 mAh/g and 1600 mAh/g respectively and still retained ∼1000 mAh/g after 80 cycles and the coulombic efficiency maintained almost 100%. The enhancement in P @rGO nanohybrid was attributed to the introduction of graphene, which led to the elimination of volume effect and the enhancement of conductively of pure red phosphorus.

  8. EG-Assisted Synthesis and Electrochemical Performance of Ultrathin Carbon-Coated LiMnPO4 Nanoplates as Cathodes in Lithium Ion Batteries

    Directory of Open Access Journals (Sweden)

    Liwei Su

    2015-01-01

    Full Text Available Ultrathin carbon-coated LiMnPO4 (ULMP/C nanoplates were prepared through an ethylene glycol- (EG- assisted pyrolysis method. Different from most of LiMnPO4/C works, the obtained ULMP/C possessed relatively small particle size (less than 50 nm in thickness and preferable carbon coating (~1 nm in thickness, 2 wt.%. As a reference, LiMnPO4/C (LMP/C composites were also fabricated via the traditional hydrothermal method. X-ray diffraction (XRD, scanning electron microscopy (SEM, transmission electron microscopy (TEM, energy dispersive X-ray spectroscopy (EDS, thermogravimetric analysis (TG, galvanostatic charge-discharge, and cyclic voltammetry (CV were performed to characterize the crystalline phase, morphology, structure, carbon content, and electrochemical behaviors of samples. The electrochemical performance of bare and carbon-coated LiMnPO4 was evaluated as cathodes in lithium ion batteries. As a result, the obtained ULMP/C nanoplates demonstrated much higher reversible capacities (110.9 mAh g−1 after 50 cycles at 0.1 C and rate performances than pure LMP and LMP/C composites. This facile and efficient EG-assisted pyrolysis method can enlighten us on exploiting advanced routes to modify active materials with ultrathin and homogeneous carbon layers.

  9. Synthesis and characterization of NiCo{sub 2}O{sub 4} nanoplates as efficient electrode materials for electrochemical supercapacitors

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Taehyun [Nanomaterials and System Lab, Department of Mechatronics Engineering, Engineering College, Jeju National University, Jeju 690-756 (Korea, Republic of); Ramadoss, Ananthakumar [Nanomaterials and System Lab, Faculty of Applied Energy System, Science and Engineering College, Jeju National University, Jeju 690-756 (Korea, Republic of); Saravanakumar, Balasubramaniam; Veerasubramani, Ganesh Kumar [Nanomaterials and System Lab, Department of Mechatronics Engineering, Engineering College, Jeju National University, Jeju 690-756 (Korea, Republic of); Kim, Sang Jae, E-mail: kimsangj@jejunu.ac.kr [Nanomaterials and System Lab, Department of Mechatronics Engineering, Engineering College, Jeju National University, Jeju 690-756 (Korea, Republic of); Nanomaterials and System Lab, Faculty of Applied Energy System, Science and Engineering College, Jeju National University, Jeju 690-756 (Korea, Republic of)

    2016-05-01

    Highlights: • NiCo{sub 2}O{sub 4} nanoplates were synthesized through a facile approach. • The NiCo{sub 2}O{sub 4} nanoplates electrode material exhibit a specific capacitance of 332 F g{sup −1} at 5 mV s{sup −1}. • The fabricated NiCo{sub 2}O{sub 4} electrode reveals 86% retention of initial capacitance after 2000 cycles. - Abstract: In the present work, NiCo{sub 2}O{sub 4} nanoplates were prepared by a facile, low temperature, hydrothermal method, followed by thermal annealing and used supercapacitor applications. The physico-chemical characterization of as-prepared materials were investigated by means of X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FT-IR) and field emission scanning electron microscopy (FE-SEM). The electrochemical measurements demonstrate that the NiCo{sub 2}O{sub 4} nanoplates electrode (NC-5) exhibits a high specific capacitance of 332 F g{sup −1} at a scan rate of 5 mV s{sup −1} and also retained about 86% of the initial specific capacitance value even after 2000 cycles at a current density of 2.5 A g{sup −1}. These results suggest that the fabricated electrode material has huge potential as a novel electrode material for electrochemical capacitors.

  10. Synthesis, pH dependent photometric and electrochemical investigation, redox mechanism and biological applications of novel Schiff base and its metallic derivatives

    Science.gov (United States)

    Rauf, Abdur; Shah, Afzal; Khan, Abdul Aziz; Shah, Aamir Hassan; Abbasi, Rashda; Qureshi, Irfan Zia; Ali, Saqib

    2017-04-01

    A novel Schiff base, 1-((2, 4-dimethylphenylimino)methyl)naphthalen-2-ol abbreviated as (HL) and its four metallic complexes were synthesized and confirmed by 1H and 13C NMR, FTIR, TGA and UV-Visible spectroscopy. Schiff base was also characterized by X-ray analysis. The photometric and electrochemical responses of all the synthesized compounds were investigated in a wide pH range. Structures of the compounds were optimized computationally for the evaluation of different physico-chemical parameters. On the basis of electrochemical results the redox mechanistic pathways of the compounds were proposed. The cytotoxicity analysis on Hela cells revealed that HL and its complexes inhibit cell growth as revealed from their IC50 values (HL):106.7 μM, (L2VO): 40.66 μM, (L2Sn): 5.92 μM, (L2Zn): 42.82 and (L2Co): 107.68 μM. The compounds were tested for anti-diabetic, triglyceride, cholesterol, anti-microbial, anti-fungal and enzyme inhibition activities. The results revealed that HL and its complexes are promising new therapeutic options as these compounds exhibit strong activity against cancer cells, diabetics, fungal and microbial inhibition.

  11. [Studies on antipeptic ulcer agents: the synthesis and structure-activity relationship analysis of heterocycle aldehyde (thio) semicarbazones and acyl hydrazones].

    Science.gov (United States)

    Guo, Z R; Yang, G Z; Chu, F M; Xu, G S; Zhang, J J; Zhang, S R; Yu, Y W

    1989-01-01

    Twenty-eight condensation products of heterocycle-alpha-carboaldehydes with N-aminooxazolidones, semicarbazides, thiosemicarbazides, aminoguanidines, aromatic hydrazides and benzoxycarbonyl hydrazide were synthesized so as to deduce the antiulcer pharmacophore or fragment of furazolidone(I), the prototype, which shows therapeutic efficacy for patients with gastric ulcer. Analysis of the SAR of the compounds indicate that the substitution of furan, thiophene, pyrrole and N-methyl pyrrole rings for the 5-nitrofuran and the cleavage of the oxazolidone ring obtain the activity to some extent. The necessary electronic density of carbonyl group of compounds is of importance. A lead structure, therefore, is derived for further optimization.

  12. Synthesis, crystal structure, antimicrobial activity and electrochemistry study of chromium(III) and copper(II) complexes based on semicarbazone Schiff base and azide ligands

    Czech Academy of Sciences Publication Activity Database

    Shaabani, B.; Khandar, A.A.; Dušek, Michal; Pojarová, Michaela; Mahmoudi, F.

    2013-01-01

    Roč. 394, JAN (2013), s. 563-568 ISSN 0020-1693 Grant - others:AV ČR(CZ) AP0701 Program:Akademická prémie - Praemium Academiae Institutional support: RVO:68378271 Keywords : antimicrobial activity * azide ligand * metal complex * Schiff base ligand * X-ray structure Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.041, year: 2013

  13. Synthesis, spectral characterization and structural studies of a novel O, N, O donor semicarbazone and its binuclear copper complex with hydrogen bond stabilized lattice

    Science.gov (United States)

    Layana, S. R.; Saritha, S. R.; Anitha, L.; Sithambaresan, M.; Sudarsanakumar, M. R.; Suma, S.

    2018-04-01

    A novel O,N,O donor salicylaldehyde-N4-phenylsemicarbazone, (H2L) has been synthesized and physicochemically characterized. Detailed structural studies of H2L using single crystal X-ray diffraction technique reveals the existence of intra and inter molecular hydrogen bonding interactions, which provide extra stability to the molecule. We have successfully synthesized a binuclear copper(II) complex, [Cu2(HL)2(NO3)(H2O)2]NO3 with phenoxy bridging between the two copper centers. The complex was characterized by elemental analysis, magnetic susceptibility and conductivity measurements, FT-IR, UV-Visible, mass and EPR spectral methods. The grown crystals of the copper complex were employed for the single crystal X-ray diffraction studies. The complex possesses geometrically different metal centers, in which the ligand coordinates through ketoamide oxygen, azomethine nitrogen and deprotonated phenoxy oxygen. The extensive intermolecular hydrogen bonding interactions of the coordinated and the lattice nitrate groups interconnect the complex units to form a 2D supramolecular assembly. The ESI mass spectrum substantiates the existence of 1:1 complex. The g values obtained from the EPR spectrum in frozen DMF suggest dx2 -y2 ground state for the unpaired electron.

  14. Synthesis, characterization, DNA interaction, antioxidant and anticancer activity of new ruthenium(II) complexes of thiosemicarbazone/semicarbazone bearing 9,10-phenanthrenequinone.

    Science.gov (United States)

    Anitha, Panneerselvam; Chitrapriya, Nataraj; Jang, Yoon Jung; Viswanathamurthi, Periasamy

    2013-12-05

    A new series of octahedral ruthenium(II) complexes supported by tridentate ligands derived from phenanthrenequinone and derivatives of thiosemicarbazide/semicarbazide and other co-ligands have been synthesized and characterized. DNA binding experiments indicated that ruthenium(II) complexes can interact with DNA through non-intercalation and the apparent binding constant value (Kb) of [RuCl(CO)(PPh₃)(L₃)] (3) at room temperature was calculated to be 2.27 × 10(3)M(-1). The DNA cleavage studies showed that the complexes have better cleavage of pBR 322 DNA. Antioxidative activity proved that the complexes have significant radical scavenging activity against free radicals. Cytotoxic activities showed that the ruthenium(II) complexes exhibited more effective cytotoxic activity against selected cancer cells. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Facile polyol synthesis of CoFe2O4 nanosphere clusters and investigation of their electrochemical behavior in different aqueous electrolytes

    Science.gov (United States)

    Malaie, K.; Ganjali, M. R.; Alizadeh, T.; Norouzi, P.

    2018-04-01

    CoFe2O4 nanosphere clusters (CFNCs) with good crystallinity were synthesized through a facile polyol process without using any surfactant or template. FESEM images show cobalt ferrite clusters with a diameter of 200-400 nm with nanospheres grown on the surface. The electrochemical behavior of the CFNCs was investigated in different electrolytes of KOH, K2SO4, and Na2SO3 in the negative potential window of - 0.3 to - 1.3 V for possible application in supercapacitor electrodes. CFNCs exhibited best performance in KOH electrolyte with a specific capacitance of 151 F g-1 in 5 mV s-1 and a cycling stability of 87% over 1000 voltammetric cycles. These studies indicate the potential application of the as-obtained CFNCs as negative electrodes in alkaline supercapacitors.

  16. Synthesis of novel tripodal-benzimidazole from 2,4,6-tris(p-formylphenoxy)-1,3,5-triazine: Structural, electrochemical and antimicrobial studies

    International Nuclear Information System (INIS)

    Koc, Ziya Erdem; Bingol, Haluk; Saf, Ahmet O.; Torlak, Emrah; Coskun, Ahmet

    2010-01-01

    Four new tripodal-benzimidazole derivatives were synthesized by Schiff base reaction between 2,4,6-tris(p-formylphenoxy)-1,3,5-triazine (TRIPOD) and different diamine derivatives. The structures of the obtained compounds were identified by FT-IR, 1 H NMR, 13 C NMR and UV-vis spectral data, thermal analysis and elemental analysis. Electrochemical behaviors of the compounds were studied by cyclic voltammetry in DMF including 0.1 M [NBu 4 ] [PF 6 ]. The voltammograms showed peaks having similar characteristics except tripodal-benzimidazole including -NO 2 derivative. In addition, their antimicrobial activities were evaluated by using the standard disk diffusion method in dimethylformamide media. The activities were determined against 4 bacteria cultures by comparing to those of gentamycin.

  17. Synthesis and Electrochemical Property of LiMn2O4Porous Hollow Nanofiber as Cathode for Lithium-Ion Batteries.

    Science.gov (United States)

    Duan, Lianfeng; Zhang, Xueyu; Yue, Kaiqiang; Wu, Yue; Zhuang, Jian; Lü, Wei

    2017-12-01

    The LiMn 2 O 4 hollow nanofibers with a porous structure have been synthesized by modified electrospinning techniques and subsequent thermal treatment. The precursors were electrospun directly onto the fluorine-doped tin oxide (FTO) glass. The heating rate and FTO as substrate play key roles on preparing porous hollow nanofiber. As cathode materials for lithium-ion batteries (LIBs), LiMn 2 O 4 hollow nanofibers showed the high specific capacity of 125.9 mAh/g at 0.1 C and a stable cycling performance, 105.2 mAh/g after 400 cycles. This unique structure could relieve the structure expansion effectively and provide more reaction sites as well as shorten the diffusion path for Li + for improving electrochemical performance for LIBs.

  18. Rhodium-catalyzed C-H bond activation for the synthesis of quinonoid compounds: Significant Anti-Trypanosoma cruzi activities and electrochemical studies of functionalized quinones.

    Science.gov (United States)

    Jardim, Guilherme A M; Silva, Thaissa L; Goulart, Marilia O F; de Simone, Carlos A; Barbosa, Juliana M C; Salomão, Kelly; de Castro, Solange L; Bower, John F; da Silva Júnior, Eufrânio N

    2017-08-18

    Thirty four halogen and selenium-containing quinones, synthesized by rhodium-catalyzed C-H bond activation and palladium-catalyzed cross-coupling reactions, were evaluated against bloodstream trypomastigotes of T. cruzi. We have identified fifteen compounds with IC 50 /24 h values of less than 2 μM. Electrochemical studies on A-ring functionalized naphthoquinones were also performed aiming to correlate redox properties with trypanocidal activity. For instance, (E)-5-styryl-1,4-naphthoquinone 59 and 5,8-diiodo-1,4-naphthoquinone 3, which are around fifty fold more active than the standard drug benznidazole, are potential derivatives for further investigation. These compounds represent powerful new agents useful in Chagas disease therapy. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

  19. Synthesis and electrochemical characterization of bimetallic ruthenium complexes with the bridging h2(s,s-1,3-butadiyne-1,4-diyl ligand

    Directory of Open Access Journals (Sweden)

    Stein Edison

    2000-01-01

    Full Text Available The bis(rutheniumalkyne complex [cis-{RuCl (bpy2(mu-CºC-}]2 (1 was obtained by treatment of 1 equiv of either 1,4-bis(trimethylsilyl-1,3-butadiyne or bis(trimetylsilylacetylene with 2 equiv of cis-[RuCl2(bpy2].2H2O, NaF and NaBF4 salts in methanol/CH2Cl2 mixture (10/1 in 52% and 35% yields, respectively. ¹H, 13C{H} NMR and principally electrochemical analyses confirmed that the same product was obtained from the two reactions. Cyclic voltammetric analyses of (1 from 0 to 1.20 V displays two one-electron quasi-reversible oxidation peaks attributed to the Ru(II/Ru(III couple. The redox processes are separated by 520 mV, indicating a significant electronic communication between the two metallic centers.

  20. Sulphur and nitrogen dual-doped mesoporous carbon hybrid coupling with graphite coated cobalt and cobalt sulfide nanoparticles: Rational synthesis and advanced multifunctional electrochemical properties.

    Science.gov (United States)

    Zhu, Anquan; Tan, Pengfei; Qiao, Lulu; Liu, Yi; Ma, Yongjin; Pan, Jun

    2018-01-01

    Doping-type carbon matrixes not only play a vital role on their electrochemical properties, but also are capable of suppressing the crush and aggregation phenomenon in the electrode reaction process for pristine metallic compound. Herein, graphite coated cobalt and cobalt sulfide nanoparticles decorating on sulphur and nitrogen dual-doped mesoporous carbon (Co@Co 9 S 8 /S-N-C) was fabricated by a combined hydrothermal reaction with pyrolysis method. Benefited from g-C 3 N 4 template and original synthetic route, as-obtained Co@Co 9 S 8 /S-N-C possessed high specific surface area (751.7m 2 g -1 ), large pore volume (1.304cm 3 g -1 ), S and N dual-doped component and relative integrated graphite skeleton, as results it was developed as decent oxygen reduction electro-catalyst and ultra-long-life Li-ion battery anode. Surprisingly, compared with commercial Pt/C, it displayed a higher half-wave potential (0.015V positive) and lower Tafel slop (66mVs -1 ), indicating its superior ORR activities. Moreover, the ultra-long-life cyclic performances were revealed for lithium ion battery, exhibiting the retention capacities of 652.1mAhg -1 after 610 cycles at 0.2Ag -1 , 432.1 and 405.7mAhg -1 at 5 and 10Ag -1 after 1000 cycles, respectively. We propose that the synergistic effect of structure and chemical component superiorities should be responsible for the remarkable electrochemical behaviors of the Co@Co 9 S 8 /S-N-C. Copyright © 2017 Elsevier Inc. All rights reserved.

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

    International Nuclear Information System (INIS)

    Pigozzi, Giancarlo; Mukherji, Debashis; Elerman, Yalçin; Strunz, Pavel; Gilles, Ralph; Hoelzel, Markus; Barbier, Bruno; Schmutz, Patrik

    2014-01-01

    Highlights: • β 1 -Ni 3 Si nanoparticles were produced by electrochemical selective phase dissolution. • A core–shell structure with ordered Ni 3 Si core and silica shell is obtained. • The ordered L1 2 crystal structure is maintained upon size reduction down to 20 nm. • Bulk Ni 3 Si is ferromagnetic below 260 K with low saturation magnetization (2 emu/g). • Nanoparticles are superparamagnetic (T B ∼ 9–11 K) with magnetization >20 emu/g. -- Abstract: Nanostructured nickel silicides find application in electronics, high-temperature alloys, electrode materials and catalysis. In this work, the effect of size reduction on the structure and magnetic properties of β 1 -Ni 3 Si intermetallic phase nanoparticles is studied. Electrochemical selective phase dissolution (ESPD) was used to produce the β 1 -Ni 3 Si nanoparticles of different sizes (from 20 to 215 nm) by extracting β 1 nano-size precipitates from two-phase Ni–Si and Ni–Si–Al precursor alloys. The extracted nanoparticles have a core–shell structure with β 1 -Ni 3 Si core and an amorphous silica shell. Particles size and shape are controlled by the composition and thermal treatment of the precursor alloys. Precipitates size is scaled without modifying the ordered L1 2 lattice structure. The bulk β 1 -Ni 3 Si is ferromagnetic below 260 K with low saturation magnetization (2 emu/g), while the core–shell Ni 3 Si/silica nanoparticles are superparamagnetic at low temperatures ( 20 emu/g at 5 T. It is suggested that weak particle magnetic moments and low magnetic anisotropy of the L1 2 structure are responsible for these properties. The shell on one hand protects the core from degradation; however the oxidation of the core/shell interface region can influence the magnetic behavior of the nano-powders

  2. Synthesis of hollow silica nanosphere with high accessible surface area and their hybridization with carbon matrix for drastic enhancement of electrochemical property

    Energy Technology Data Exchange (ETDEWEB)

    Alam, Mohammad Mydul; Yamahana, Haruki [Department of Chemistry, Faculty of Science and Engineering, Saga University, 1 Honjo-machi, Saga 840-8502 (Japan); Bastakoti, Bishnu Prasad [World Premier International (WPI) Research Center for Materials Nanoarchitectonics (MANA), National Institute for Materials Science - NIMS, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Luitel, Hom Nath; Zhao, Wenwen [Department of Chemistry, Faculty of Science and Engineering, Saga University, 1 Honjo-machi, Saga 840-8502 (Japan); Yamauchi, Yusuke [World Premier International (WPI) Research Center for Materials Nanoarchitectonics (MANA), National Institute for Materials Science - NIMS, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Department of Nanoscience and Nanoengineering, Faculty of Science and Engineering, Waseda University, 3-4-1 Okubo, Shinjuku, Tokyo 169-8555 (Japan); Watari, Takanori; Noguchi, Hideyuki [Department of Chemistry, Faculty of Science and Engineering, Saga University, 1 Honjo-machi, Saga 840-8502 (Japan); Nakashima, Kenichi, E-mail: nakashik@cc.saga-u.ac.jp [Department of Chemistry, Faculty of Science and Engineering, Saga University, 1 Honjo-machi, Saga 840-8502 (Japan)

    2014-09-30

    Highlights: • Hollow silica nanosphere with large void space and high surface area is synthesized. • Carbon was doped into silica layer through glucose solution and resulting carbon/silica composite drastically enhanced electrochemical property. • Combination of core–shell–corona micelle template and doping method could be a new platform for developing functional materials. - Abstract: Hollow silica nanospheres with high accessible surface area have been synthesized by using core–shell–corona polymeric micelle of poly (styrene-b-2-vinyle pyridine-b-ethylene oxide) (PS45k-PVP26k-PEO82k) as a template. The size of the template polymeric micelle depends on the pH of the solution, i.e. ≈100 nm at pH 7 whereas ≈300 nm at pH 4. The enlarged size of the micelle is possibly due to the protonation of the PVP block, which also serves as reaction sites for silica precursor. The size of the obtained silica nanosphere measured with transmission electron microscope (TEM) is around ≈70 nm and shell thickness is ≈20 nm. Fourier transformed infrared spectroscopy (FTIR) data confirms that the polymer template is completely removed during calcination. Conductive carbon is doped into the silica nanosphere through glucose solution followed by hydrothermal treatment and pyrolysis. It is found that the electrochemical performance and stability of the silica nanosphere is dramatically enhanced after carbon doping. The combined strategy of the core–shell–corona micelle as template and carbon doping could represent a new platform for the researchers to develop functional nanomaterials.

  3. Synthesis and electrochemical performance of Li2FeSiO4/C/carbon nanosphere composite cathode materials for lithium ion batteries

    International Nuclear Information System (INIS)

    Yang, Jinlong; Kang, Xiaochun; Hu, Lin; Gong, Xue; He, Daping; Peng, Tao; Mu, Shichun

    2013-01-01

    Highlights: •The Li 2 FeSiO 4 /C/CNS was prepared by effective double-carbon composite route. •The CNS as the conductivity belt connects the Li 2 FeSiO 4 /C particles. •The samples have a high capacity and excellent cyclic and rate performance. -- Abstract: Li 2 FeSiO 4 /C/carbon nanosphere (CNS) composites as cathode materials for lithium-ion batteries were synthesized by a simple hydro-chemical method. The double-carbon structural design of glucose pyrolysis-carbon (C) and CNS improved electrochemical performance of the composite where the CNS can build conductivity belts to connect the Li 2 FeSiO 4 /C particles and to favor electronic transmission. The exchange current density and the diffusion coefficient of lithium ions with the composite were 0.208 mA cm −2 and 1.06E−11 cm 2 S −1 , respectively, which were much larger than that of conventional Li 2 FeSiO 4 /C composite cathode materials (i = 0.131 mA cm −2 , D Li = 4.69E−12 cm 2 S −1 ). The electrochemical test results showed that the discharge capacity of 164.7 mA h g −1 could be obtained, and especially, after 60 cycles, 98.4% of the initial discharge capacity remained at 0.1 C of galvanostatic discharge in the potential range of 1.5–4.8 V (vs. Li/Li + ). In addition, the discharge capacity of 92.4 mA h g −1 at 5 C was easily recovered to 159.8 mA h g −1 at 0.1 C

  4. Synthesis and electrocatalytic effect of Ag@Pt core-shell nanoparticles supported on reduced graphene oxide for sensitive and simple label-free electrochemical aptasensor.

    Science.gov (United States)

    Mazloum-Ardakani, Mohammad; Hosseinzadeh, Laleh; Taleat, Zahra

    2015-12-15

    Bimetallic Ag@Pt core-shell nanoparticles supported on reduced graphene oxide nanosheets (Ag@Pt-GRs) was synthesized and used as novel desirable sensor platform and electrocatalyst for catechol as probe in aptasensor. Gold screen-printed electrodes modified with Ag@Pt-GRs and applied to advance enzyme-free and label-free electrochemical aptasensor for detection of protein biomarker tumor necrosis factor-alpha (TNF-α). The morphology of the Ag@Pt-GRs could be characterized by transmission electron microscopy, X-ray diffraction and UV-vis spectra. The results showed that these nanocomposite exhibited attractive electrocatalytic activity and also yielded large surface area, which improve the amount of immobilized TNF-α aptamer. Due to the excellent electrocatalytic activity of Ag@Pt-GRs towards the oxidation of catechol, determination of TNF-α antigen was based on its obstruction to the electrocatalytic oxidation of catechol by Ag@Pt-GRs after binding to the surface of electrode through interaction with the aptamer. The calibration curve was obtained by differential pulse voltammetry and square wave voltammetry. Under optimum conditions, the results demonstrated that this electrochemical aptasensor possessed a dynamic range from 0.0 pg/mL to 60 pg/mL with a low detection limit of 2.07 pg/mL for TNF-α. The analytical usefulness of the aptasensor was finally demonstrated analyzing serum samples. The simple fabrication method, high sensitivity, specificity, good reproducibility and stability as well as acceptable accuracy for TNF-α detection in human serum samples are the main advantages of this aptasensor, which might have broad applications in protein diagnostics and bioassay. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Synthesis of core/shell ZnO/ZnSe nanowires using novel low cost two-steps electrochemical deposition technique

    Energy Technology Data Exchange (ETDEWEB)

    Ghoul, M., E-mail: ghoulmed2009@yahoo.fr [Laboratoire Photovoltaïque, Centre de Recherches et des Technologies de l' Energie Technopole BorjCedria, Bp 95, Hammammlif 2050 (Tunisia); Braiek, Z. [Laboratoire Photovoltaïque, Centre de Recherches et des Technologies de l' Energie Technopole BorjCedria, Bp 95, Hammammlif 2050 (Tunisia); Brayek, A. [Laboratoire Photovoltaïque, Centre de Recherches et des Technologies de l' Energie Technopole BorjCedria, Bp 95, Hammammlif 2050 (Tunisia); ITODYS, Université Paris Diderot, Sorbonne Paris Cité, CNRS UMR – 7086, 75205 Paris (France); Ben Assaker, I.; Khalifa, N.; Ben Naceur, J.; Souissi, A.; Lamouchi, A. [Laboratoire Photovoltaïque, Centre de Recherches et des Technologies de l' Energie Technopole BorjCedria, Bp 95, Hammammlif 2050 (Tunisia); Ammar, S. [ITODYS, Université Paris Diderot, Sorbonne Paris Cité, CNRS UMR – 7086, 75205 Paris (France); Chtourou, R. [Laboratoire Photovoltaïque, Centre de Recherches et des Technologies de l' Energie Technopole BorjCedria, Bp 95, Hammammlif 2050 (Tunisia)

    2015-10-25

    This work highlights the original use of a two-step electrochemical deposition protocol to grow ZnO/ZnSe core/shell nanowires on a Sn-doped In{sub 2}O{sub 3} (ITO)/glass substrate. The good alignment of the nanowires is verified by the scanning electron microscopy characterization technique in addition to the surface roughness after the ZnSe electrodeposition on the ZnO nanowires lateral facets. The X-ray diffraction patterns and Raman spectra allow estimating that ZnO has grown along the wurtzite (W) structure c-axis. The presence of the type-II interfacial transition between the valence band of ZnSe and the conduction band of ZnO was confirmed by UV–visible spectroscopy. It was proved that the absorbed energy of the developed nanostructures is extended to the near infrared which is well recommended for the photovoltaic applications. - Graphical abstract: Fabrication of the ZnO–ZnSe core–shell nanowires through a solution based all-electrochemical approach, and their application as photoanodes in photoelectrochemical water splitting cells. - Highlights: • Deposition of ZnO/ZnSe nanowires by two steps electrodeposition method. • The morphology studies show the formation of ZnO/ZnSe core/Shell nanowires. • XRD and Raman spectroscopy confirm the presence of the wurtzite ZnO and blende ZnSe junction. • Optical properties demonstrate the evidence type-II interfacial transition between the two semiconductors.

  6. Synthesis and electrochemical properties of Fe{sub 3}O{sub 4}@MOF core-shell microspheres as an anode for lithium ion battery application

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Xuemin; Gao, Ge [Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Ministry-of-Education Key Laboratory for Synthesis and Applications of Organic Functional Molecules, Hubei University, Wuhan 430062 (China); Yan, Dongwei, E-mail: dwyan@iccas.ac.cn [Advance Technology & Materials Co. Ltd., China Iron & Steel Research Institute Group, No. 76 Xueyuan Nanlu, Haidian District, Beijing 100081 (China); Feng, Chuanqi, E-mail: cfeng@hubu.edu.cn [Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Ministry-of-Education Key Laboratory for Synthesis and Applications of Organic Functional Molecules, Hubei University, Wuhan 430062 (China)

    2017-05-31

    Highlights: • Fe{sub 3}O{sub 4} particles are encapsulated by HKUST-1 to form core-shell microspheres composite. • The composite exhibits outstanding electrochemical performances as a novel anode. • The typical approach can be used to prepare some novel electrode materials. - Abstract: The Fe{sub 3}O{sub 4}@MOF composite with a microspheric core and a porous metal-organic framework (MOF HKUST-1) shell has been successfully synthesized utilizing a versatile Layer-by-Layer (LBL) assembly method. The structure was identified by X-ray diffraction (XRD), and the morphology was investigated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques. The Fe{sub 3}O{sub 4}@MOF composite exhibited outstanding electrochemical properties when it was used as an anode material for lithium ion batteries (LIBs). After 100 discharge-charge cycles at a current density of 100 mA g{sup −1}, the reversible capacity of Fe{sub 3}O{sub 4}@MOF could maintain ∼1002 mAh g{sup −1}, which was much higher than that of the bare Fe{sub 3}O{sub 4} counterpart (696 mAh g{sup −1}). Moreover, load the current density as high as 2 A g{sup −1} (after 70 cycles at the current density step increased from 0.1 to 2 A g{sup −1}), it still delivered a reversible capacity of ∼429 mAh g{sup −1}. The results demonstrate that the cycling stability of Fe{sub 3}O{sub 4} as an anode could be significantly improved by coating Cu{sub 3}(1,3,5-benzenetricarboxylate){sub 2} (HKUST-1). This strategy may offer new route to prepare other composite materials using different particles and suitable Metal-organic frameworks (MOFs) for LIBs application.

  7. ELECTROCHEMICAL BEHAVIOUR OF ENVIRONMENTALLY ...

    African Journals Online (AJOL)

    dell

    ABSTRACT. Electrochemical behaviour of Aloe secundiflora on carbon steel corrosion control in neutral and aerated soft water solutions have been investigated using electrochemical impedance spectroscopy and Tafel polarization techniques. The investigation was performed at different inhibitor concentrations under ...

  8. Separators for electrochemical cells

    Energy Technology Data Exchange (ETDEWEB)

    Carlson, Steven Allen; Anakor, Ifenna Kingsley; Farrell, Greg Robert

    2018-01-16

    Provided are separators for use in an electrochemical cell comprising (a) an inorganic oxide and (b) an organic polymer, wherein the inorganic oxide comprises organic substituents. Also provided are electrochemical cells comprising such separators.

  9. Electrochemical Hydrogen Refrigerator

    Data.gov (United States)

    National Aeronautics and Space Administration — The goal is to develop and test a 1 W at 20K Joule‐Thomson cryocooler using an electrochemical compressor. A Joule Thomson refrigerator based on electrochemical...

  10. Synthesis, electrochemical investigation and structural analysis of doped Li[Ni0.6Mn0.2Co0.2-xMx]O2 (x = 0, 0.05; M = Al, Fe, Sn) cathode materials

    Science.gov (United States)

    Eilers-Rethwisch, Matthias; Winter, Martin; Schappacher, Falko Mark

    2018-05-01

    Layered Ni-rich Li[Ni0.6Mn0.2Co0.2-xMx]O2 cathode materials (x = 0, 0.05; M = Al, Fe, Sn) are synthesized via a co-precipitation synthesis route and the effect of dopants on the structure and electrochemical performance is investigated. All synthesized materials show a well-defined layered structure of the hexagonal α-NaFeO2 phase investigated by X-ray diffraction (XRD). Undoped LiNi0.6Mn0.2Co0.2O2 exhibits a discharge capacity of 170 mAh g-1 in Li-metal 2032 coin-type cells. Doped materials reach lower capacities between 145 mAh g-1 for Al and 160 mAh g-1 for Sn. However, all doped materials prolong the cycle life by up to 20%. Changes of the lattice parameter before and after delithiation yield information about structural stability. A smaller repulsion of the transition metal layer during delithiation in the Sn-doped material leads to a smaller expansion of the unit cell, which results in enhanced structural stability of the material. The improved structural stability of Sn-doped NMC cathode active material is proven by thermal investigations with the help of Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis (TGA).

  11. Synthesis, Spectroscopy, Theoretical, and Electrochemical Studies of Zn(II, Cd(II, and Hg(II Azide and Thiocyanate Complexes of a New Symmetric Schiff-Base Ligand

    Directory of Open Access Journals (Sweden)

    Morteza Montazerozohori

    2013-01-01

    Full Text Available Synthesis of zinc(II/cadmium(II/mercury(II thiocyanate and azide complexes of a new bidentate Schiff-base ligand (L with general formula of MLX2 (M = Zn(II, Cd(II, and Hg(II in ethanol solution at room temperature is reported. The ligand and metal complexes were characterized by using ultraviolet-visible (UV-visible, Fourier transform infrared (FT-IR, 1H- and 13C-NMR spectroscopy and physical characterization, CHN analysis, and molar conductivity. 1H- and 13C-NMR spectra have been studied in DMSO-d6. The reasonable shifts of FT-IR and NMR spectral signals of the complexes with respect to the free ligand confirm well coordination of Schiff-base ligand and anions in an inner sphere coordination space. The conductivity measurements as well as spectral data indicated that the complexes are nonelectrolyte. Theoretical optimization on the structure of ligand and its complexes was performed at the Becke’s three-parameter hybrid functional (B3 with the nonlocal correlation of Lee-Yang-Parr (LYP level of theory with double-zeta valence (LANL2DZ basis set using GAUSSIAN 03 suite of program, and then some theoretical structural parameters such as bond lengths, bond angles, and torsion angles were obtained. Finally, electrochemical behavior of ligand and its complexes was investigated. Cyclic voltammograms of metal complexes showed considerable changes with respect to free ligand.

  12. Hierarchical structured carbon derived from bagasse wastes: A simple and efficient synthesis route and its improved electrochemical properties for high-performance supercapacitors

    Science.gov (United States)

    Feng, Haobin; Hu, Hang; Dong, Hanwu; Xiao, Yong; Cai, Yijin; Lei, Bingfu; Liu, Yingliang; Zheng, Mingtao

    2016-01-01

    Bagasse-derived hierarchical structured carbon (BDHSC) with tunable porosity and improved electrochemical performance is prepared via simple and efficient hydrothermal carbonization combined with KOH activation. Experimental results show that sewage sludge acts as a cheap and efficient structure-directing agent to regulate the morphology, adjust the porosity, and thus improve the supercapacitive performance of BDHSC. The as-resulted BDHSC exhibits an interconnected framework with high specific surface area (2296 m2 g-1), high pore volume (1.34 cm3 g-1), and hierarchical porosity, which offer a more favorable pathway for electrolyte penetration and transportation. Compared to the product obtained from bagasse without sewage sludge, the unique interconnected BDHSC exhibits enhanced supercapacitive performances such as higher specific capacitance (320 F g-1), and better rate capability (capacitance retention over 70.8% at a high current density of 50 A g-1). Moreover, the BDHSC-based symmetric supercapacitor delivers a maximum energy density of over 20 Wh kg-1 at 182 W kg-1 and presents an excellent long-term cycling stability. The developed approach in the present work can be useful not only in production of a variety of novel hierarchical structured carbon with promising applications in high-performance energy storage devices, but also in high-value utilization of biomass wastes and high-ash-content sewage sludge.

  13. Solution Process Synthesis of High Aspect Ratio ZnO Nanorods on Electrode Surface for Sensitive Electrochemical Detection of Uric Acid

    Science.gov (United States)

    Ahmad, Rafiq; Tripathy, Nirmalya; Ahn, Min-Sang; Hahn, Yoon-Bong

    2017-04-01

    This study demonstrates a highly stable, selective and sensitive uric acid (UA) biosensor based on high aspect ratio zinc oxide nanorods (ZNRs) vertical grown on electrode surface via a simple one-step low temperature solution route. Uricase enzyme was immobilized on the ZNRs followed by Nafion covering to fabricate UA sensing electrodes (Nafion/Uricase-ZNRs/Ag). The fabricated electrodes showed enhanced performance with attractive analytical response, such as a high sensitivity of 239.67 μA cm-2 mM-1 in wide-linear range (0.01-4.56 mM), rapid response time (~3 s), low detection limit (5 nM), and low value of apparent Michaelis-Menten constant (Kmapp, 0.025 mM). In addition, selectivity, reproducibility and long-term storage stability of biosensor was also demonstrated. These results can be attributed to the high aspect ratio of vertically grown ZNRs which provides high surface area leading to enhanced enzyme immobilization, high electrocatalytic activity, and direct electron transfer during electrochemical detection of UA. We expect that this biosensor platform will be advantageous to fabricate ultrasensitive, robust, low-cost sensing device for numerous analyte detection.

  14. Synthesis, electrochemical, spectrophotometric and potentiometric studies of two azo-compounds derived from 4-amino-2-methylquinoline in ethanolic-aqueous buffered solutions

    Energy Technology Data Exchange (ETDEWEB)

    El-Attar, Mona A.; Ghoneim, Mohamed M. [Analytical Chemistry Research Unit, Chemistry Department, Tanta University (Egypt); Ismail, Iqbal M., E-mail: maema.2011@yahoo.com [Chemistry Department, Faculty of Science, King Abdul Aziz University, Jeddah (Saudi Arabia)

    2012-08-15

    Two azo-compounds, 2-methyl-4-(5-amino-2-hydroxy-phenylazo)-quinoline (2) and 2-methyl-4-(2-hydroxy-5-nitrophenylazo)-quinoline, derived from 4-amino-2-methylquinoline were synthesized. Their chemical structures were characterized and confirmed by means of elemental chemical analysis, infrared (IR) spectroscopy, {sup 1}H nuclear magnetic resonance (NMR) and mass spectrometry (MS). The electrochemical behavior of the starting compound (4-amino-2-methylquinoline) and of the two synthesized azo-derivatives was studied at the mercury electrode in the B-R universal buffer at various pH values (2-11.5) containing 40% (v/v) ethanol using dc-polarography, cyclic voltammetry and controlled-potential coulometry. Their electrode reaction pathways were elucidated and discussed. The dissociation constants (pKa) of the examined compounds, stability constants and stoichiometry of their complexes in solution with some transition metal ions (Co(II), Ni(II), Cu(II), La(III) and UO{sup 2+}{sub 2}) were determined. (author)

  15. Ruthenium(II) bipyridine complexes bearing quinoline-azoimine (NN'N″) tridentate ligands: synthesis, spectral characterization, electrochemical properties and single-crystal X-ray structure analysis.

    Science.gov (United States)

    Al-Noaimi, Mousa; Abdel-Rahman, Obadah S; Fasfous, Ismail I; El-khateeb, Mohammad; Awwadi, Firas F; Warad, Ismail

    2014-05-05

    Four octahedral ruthenium(II) azoimine-quinoline complexes having the general molecular formula [Ru(II)(L-Y)(bpy)Cl](PF6) {L-Y=YC6H4N=NC(COCH3)=NC9H6N, Y=H (1), CH3 (2), Br (3), NO2 (4) and bpy=2,2'-bipyrdine} were synthesized. The azoimine-quinoline based ligands behave as NN'N″ tridentate donors and coordinated to ruthenium via azo-N', imine-N' and quinolone-N″ nitrogen atoms. The composition of the complexes has been established by elemental analysis, spectral methods (FT-IR, electronic, (1)H NMR, UV/Vis and electrochemical (cyclic voltammetry) techniques. The crystal structure of complex 1 is reported. The Ru(II) oxidation state is greatly stabilized by the novel tridentate ligands, showing Ru(III/II) couples ranging from 0.93-1.27 V vs. Cp2Fe/Cp2Fe(+). The absorption spectrum of 1 in dichloromethane was modeled by time-dependent density functional theory (TD-DFT). Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Facile synthesis of the N-doped graphene/nickel oxide with enhanced electrochemical performance for rechargeable lithium-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Chuanning, E-mail: yangcn1988@outlook.com [Key Laboratory for Anisotropy and Texture of Materials of Ministry of Education, Northeastern University, Shenyang, Liaoning 110819 (China); Qing, Yongquan; An, Kai [Key Laboratory for Anisotropy and Texture of Materials of Ministry of Education, Northeastern University, Shenyang, Liaoning 110819 (China); Zhang, Zefei; Wang, Linshan [College of Science, Northeastern University, Shenyang, Liaoning 110819 (China); Liu, Changsheng, E-mail: csliu@mail.neu.edu.cn [Key Laboratory for Anisotropy and Texture of Materials of Ministry of Education, Northeastern University, Shenyang, Liaoning 110819 (China)

    2017-07-01

    The nitrogen-doped graphene/NiO nanohybrids with a hierarchical structure have been successfully synthesized by a one-step hydrothermal route assisted by microwave treatment. The as-obtained products were characterized by scanning electron microscopy, high-resolution transmission microscopy, powder X-ray diffraction, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and thermogravimetric analysis. The nitrogen-doped graphene/NiO electrodes exhibit an enhanced electrochemical performance. The initial discharge capacity can reach 1737 mAh g{sup -1} at the current density of 0.1 A g{sup -1}. Significantly, the nanocomposites anodes also display a relatively high reversible capacity of 1095 mAh g{sup -1} at the current density of 0.3 A g{sup -1} after 100 cycles. Herein, the nitrogen-doped graphene/NiO possesses electrodes enormous potential as the anode materials for lithium ion batteries. - Highlights: • The nitrogen-doped graphene/NiO nanohybrids have been successfully synthesized. • Microwave treatment may enhance conductivity and capacity of electrodes. • The hierarchical structure will help to improve the stability of the electrodes. • The reversible capacity of electrodes can reach 1095 mAh g{sup -1} over 100 cycles.

  17. Conjugated Polymers Containing BODIPY and Fluorene Units for Sensitive Detection of CN− Ions: Site-Selective Synthesis, Photo-Physical and Electrochemical Properties

    Directory of Open Access Journals (Sweden)

    Tian He

    2017-10-01

    Full Text Available Conjugated polymers containing distinct molecular units are expected to be very interesting because of their unique properties endowed by these units and the formed conjugated polymers. Herein, four new conjugated copolymers based on fluorene and 4,4’-difluoro-4-bora-3a,4a-diaza-s-indacene (BODIPY have been designed and synthesized via Sonogashira polymerization. The fluorene unit was attached to the 3,5- or 2,6-positions of BODIPY by ethynylenes or p-diacetylenebenzene. The obtained polymers show good thermal stability and broad absorption in the wavelength range from 300 to 750 nm. The effects of site-selective copolymerization and conjugation length along the polymer backbone on the optoelectronic and electrochemical properties of these copolymers were systematically studied by UV-Vis spectroscopy, photoluminescence (PL and cyclic voltammetry. Besides, it is found that the BODIPY-based copolymers exhibit selectively sensitive responses to cyanide anions, resulting in obvious change of UV-Vis absorption spectra and significant fluorescence quenching of the polymers among various common anions.

  18. A novel electrochemical synthesis of poly-3-methylthiophene-gamma-cyclodextrin film Application for the analysis of chlorpromazine and some neurotransmitters.

    Science.gov (United States)

    Bouchta, Dounia; Izaoumen, Nissrin; Zejli, Hanane; El Kaoutit, Mohamed; Temsamani, Khalid R

    2005-05-15

    Gamma-cyclodextrin is an eight glucose unit conical structure, which possesses a hydrophobic internal cavity exhibiting supramolecular complexing properties and a hydrophilic exterior due to the presence of hydroxyl groups. In this work, we have synthesized for the first time a functionalized stable film of poly-3-methylthiophene combined with gamma-cyclodextrin (P3MT/gamma-CD) in tetrabutylammonium hexafluorophosphate/acetonitrile solution. A potentiostatic mode was employed for the film growth. Cyclic voltammetry and electrochemical impedance spectroscopy were used for the characterization of the new film. The resulting conducting polymer sensor offers interesting analytical performances such as: (a) fast and linear responses towards the neurotransmitters dopamine and l-dopa towards the neuroleptic chlorpromazine with low detection limits of 2 x 10(-7), 10(-6), and 10(-7)M, respectively, and (b) simultaneous detection and well-resolved signals between the compounds of interest and ascorbic acid. To the best of our knowledge, these LOD are among the lowest found in the literature. Optimization of parameters such as interference effect, perm-selectivity, and mechanical stability of the sensor are discussed.

  19. Synthesis and electrochemical behavior of nanosized LiNi1-xCa xO2 cathode materials for high voltage secondary lithium-ion cells

    International Nuclear Information System (INIS)

    Sathiyamoorthi, R.; Vasudevan, T.

    2007-01-01

    A new class of LiNi 1-x Ca x O 2 (x = 0.0, 0.1, 0.2, 0.3 and 0.5) layered oxide materials has been synthesized by a simple low temperature solid-state route with mixed nitrates/urea with glycerol as the starting materials. First we have taken TG/DTA for observing the phase transformations of LiNi 0.9 Ca 0.1 O 2 . The structure of the synthesized oxides was analyzed using X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) to identify the crystal structure and cation environment, respectively. The synthesized ceramic oxide battery materials were examined by using transmission electron microscope (TEM), scanning electron microscope (SEM) analysis to determine the particle size, nature and morphological structure. SEM with energy dispersive X-ray spectroscopic analysis (EDAX) analysis was carried out to explore the composition of the prepared materials. The electrochemical performance of LiNi 1-x Ca x O 2 electrodes was analyzed using cyclic voltammetry (CV) and galvanostatic charge-discharge cycling studies in the voltage range 3.0-4.5 V. Electrode made with cathode active material, acetylene black and poly(vinylidene difluoride) yield a discharge capacity of 178.1 mAh g -1 (x = 0.2) with good specific capacity over several charge-discharge cycles. These results have been also supported by cyclic voltammograms

  20. Electrochemical synthesis, characterization and electrochromic properties of a copolymer based on 1,4-bis(2-thienyl)naphthalene and pyrene

    Science.gov (United States)

    Wang, Bin; Zhao, Jinsheng; Cui, Chuansheng; Wang, Min; Wang, Zhong; He, Qingpeng

    2012-05-01

    Electrochemical copolymerization of 1,4-bis(2-thienyl)naphthalene (BTN) with pyrene is carried out in acetonitrile (ACN) solution containing sodium perchlorate (NaClO4) as a supporting electrolyte. Characterizations of the resulting copolymer P(BTN-co-pyrene) are performed by cyclic voltammetry (CV), UV-vis spectroscopy, Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). The P(BTN-co-pyrene) film has distinct electrochromic properties and exhibits three different colors (yellowish green, green and blue) under various potentials. Maximum contrast (ΔT%) and response time of the copolymer film are measured as 37.8% and 1.71 s at 687 nm. An electrochromic device (ECD) based on P(BTN-co-pyrene) and poly(3,4-ethylenedioxythiophene) (PEDOT) is constructed and characterized. Neutral state of device shows green color while oxidized state reveals blue color. This ECD shows a maximum optical contrast (ΔT%) of 24.4% with a response time of 0.43 s at 635 nm. The coloration efficiency (CE) of the device is calculated to be 349 cm2 C-1 at 635 nm. In addition, the ECD also has satisfactory optical memories and redox stability.

  1. New Cu (II), Co(II) and Ni(II) complexes of chalcone derivatives: Synthesis, X-ray crystal structure, electrochemical properties and DFT computational studies

    Science.gov (United States)

    Tabti, Salima; Djedouani, Amel; Aggoun, Djouhra; Warad, Ismail; Rahmouni, Samra; Romdhane, Samir; Fouzi, Hosni

    2018-03-01

    The reaction of nickel(II), copper(II) and cobalt(II) with 4-hydroxy-3-[(2E)-3-(1H-indol-3-yl)prop-2-enoyl]-6-methyl-2H-pyran-2-one (HL) leads to a series of new complexes: Ni(L)2(NH3), Cu(L)2(DMF)2 and Co(L)2(H2O). The crystal structure of the Cu(L)2(DMF)2 complex have been determined by X-ray diffraction methods. The Cu(II) lying on an inversion centre is coordinated to six oxygen atoms forming an octahedral elongated. Additionally, the electrochemical behavior of the metal complexes were investigated by cyclic voltammetry at a glassy carbon electrode (GC) in CH3CN solutions, showing the quasi-reversible redox process ascribed to the reduction of the MII/MI couples. The X-ray single crystal structure data of the complex was matched excellently with the optimized monomer structure of the desired compound; Hirschfeld surface analysis supported the packed crystal lattice 3D network intermolecular forces. HOMO/LUMO energy level and the global reactivity descriptors quantum parameters are also calculated. The electrophilic and nucleophilic potions in the complex surface are theoretically evaluated by molecular electrostatic potential and Mulliken atomic charges analysis.

  2. Synthesis and Biochemical effects of magnetite nanoparticle by surfactant-free electrochemical method in an aqueous system:the current density effect

    Directory of Open Access Journals (Sweden)

    Mousa Aliahmad

    2016-07-01

    Full Text Available Obejective(s: In this research, magnetite nanoparticles with an average size of 23-36 nm were successfully synthesized via surfactant-free electrochemical method using iron as the anode and water as the electrolyte in a closed aqueous system in the presence of NaOH at room temperature. Methods: The effect of the current density on product formation and particle size was investigated. Particle size was controlled by adjusting the current density. It was found that particle size decreases by decreasing the current density. In addition, the effect of current density  on the structural and optical properties of nanostructures were studied by X-ray diffraction, Field emission scanning electron microscopy, Fourier transformed infrared, and vibrating sample magnetometer techniques.  Results: The results obtained from the magnetization property study of samples at room temperature showed coactivity and saturation manetization of 0-100 Oe and 27.2- 40.5 emu. g-1, respectively. Finally, the results of biological activity study of nanoparticles on liver and kidney function in male wistar rats demonstrated that oral administration of NPs caused significant alterations to the levels of aspartate transaminase, alanine transaminase, and alkaline phosphatase in serum. Conclusions: No significant changes were detected in the groups treated with 10 and 100 ppm/ day nanostructure (P>0.05. There was a significant increase in the serum level of creatinine and blood urea nitrogen level (p

  3. A new 3D POMOF based on CuI/CuII-bis(triazole) complexes and BW12 Keggin polyoxoanions: Synthesis, characterization and electrochemical properties

    Science.gov (United States)

    Zhang, Yanjun; Fu, Xin; Zhang, Chunjing; Pang, Hainjun; Ma, Huiyuan; Zhao, Xi; Wang, Cheng

    2018-02-01

    A novel organic-inorganic hybrid compound, {[CuI(btpe)2][CuII2(H2O)2(btpe)2][BW12O40]}·2H2O, (btpe = 1,5-bis(1,2,4-triazol-1-yl)pentane) (1) has been synthesized by hydrothermal reaction, and characterized by elemental analyses, IR spectroscopy, TG and single X-ray diffraction. Compound 1 is composed of α-Keggin type [BW12O40]5- (BW12) polyoxoanions and copper-btpe complexes. The copper-btpe complexes are stagger-packed to form an open framework containing the two kinds of channels with parallelogram-like apertures, in which the BW12 guests are encapsulated into the bigger channels. The electrochemical studies show that 1 has a good electrocatalytic activity towards reduction of hydrogen peroxide (H2O2), thanking to its special porous POMOF structure. The molecular design of 1 not only generates a new POMOF, but also opens a new avenue to the electrocatalytic materials.

  4. In situ synthesis of ceria nanoparticles in the ordered mesoporous carbon as a novel electrochemical sensor for the determination of hydrazine

    International Nuclear Information System (INIS)

    Liu, Yue; Li, Yijun; He, Xiwen

    2014-01-01

    Highlights: • CeO 2 –OMC composites were prepared via a hydrothermal method. • CeO 2 –OMC had electrocatalytic ability to oxidation of hydrazine. • The sensor had high sensitivity, excellent stability and reproducibility. • The sensor was successfully employed to detect hydrazine in real water samples. - Abstract: A novel ceria (CeO 2 )–ordered mesoporous carbon (OMC) modified electrode for the sensitive amperometric determination of hydrazine was reported. CeO 2 –OMC composites were synthesized via a hydrothermal method at a relatively low temperature (180 °C) and characterized by scanning electron microscopy (SEM), transmission electron microcopy (TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The CeO 2 –OMC modified glassy carbon electrode was characterized by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) and indicated good electrocatalytic effect to the oxidation of hydrazine. Under the optimized conditions, the present sensor could be used to measure hydrazine in wide linear range from 40 nM to 192 μM (R 2 = 0.999) with a low detection limit of 12 nM (S/N = 3). Additionally, the sensor has been successfully applied to detect hydrazine in real water samples and the recoveries were between 98.2% and 105.6%. Eventually, the sensor exhibited an excellent stability and reproducibility as a promising method for determination of hydrazine

  5. In situ synthesis of ceria nanoparticles in the ordered mesoporous carbon as a novel electrochemical sensor for the determination of hydrazine

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Yue [College of Chemistry, Nankai University, 94 WeiJin Road, Tianjin 300071 (China); Li, Yijun, E-mail: yijunli@nankai.edu.cn [Collaborative Innovation Center of Chemical Science and Engineering (Tianjin), Tianjin 300071 (China); College of Chemistry, Nankai University, 94 WeiJin Road, Tianjin 300071 (China); He, Xiwen [College of Chemistry, Nankai University, 94 WeiJin Road, Tianjin 300071 (China)

    2014-03-01

    Highlights: • CeO{sub 2}–OMC composites were prepared via a hydrothermal method. • CeO{sub 2}–OMC had electrocatalytic ability to oxidation of hydrazine. • The sensor had high sensitivity, excellent stability and reproducibility. • The sensor was successfully employed to detect hydrazine in real water samples. - Abstract: A novel ceria (CeO{sub 2})–ordered mesoporous carbon (OMC) modified electrode for the sensitive amperometric determination of hydrazine was reported. CeO{sub 2}–OMC composites were synthesized via a hydrothermal method at a relatively low temperature (180 °C) and characterized by scanning electron microscopy (SEM), transmission electron microcopy (TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The CeO{sub 2}–OMC modified glassy carbon electrode was characterized by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) and indicated good electrocatalytic effect to the oxidation of hydrazine. Under the optimized conditions, the present sensor could be used to measure hydrazine in wide linear range from 40 nM to 192 μM (R{sup 2} = 0.999) with a low detection limit of 12 nM (S/N = 3). Additionally, the sensor has been successfully applied to detect hydrazine in real water samples and the recoveries were between 98.2% and 105.6%. Eventually, the sensor exhibited an excellent stability and reproducibility as a promising method for determination of hydrazine.

  6. Stepwise synthesis, characterization, and electrochemical properties of ordered mesoporous carbons containing well-dispersed Pt nanoparticles using a functionalized template route

    International Nuclear Information System (INIS)

    Liu, Shou-Heng; Chen, Shih-Che

    2011-01-01

    A stepwise method is described for the accurately controlled growth of Pt nanoparticles supported on ordered mesoporous carbons (Pt-OMC) by the nanocasting of carbon and metal precursors in the pore channels of mesoporous silicas functionalized with Si-H groups. Results obtained from N 2 adsorption/desorption isotherms and transmission electron microscopy showed well-dispersed Pt nanoparticles (2-3 nm) on Pt-OMC with high surface area (837 m 2 g -1 ) and regular pore channels (2.9 nm), which facilitate reactant/product diffusion. X-ray diffraction and X-ray photoelectron spectroscopy indicated that Pt nanoparticles in the Pt-OMC sample were mostly present in the metallic form of a face-centered cubic (fcc) crystalline structure. The Pt-OMC catalyst was found to have superior electrocatalytic properties during oxygen reduction reaction as compared to typical commercial electrocatalysts. - Graphical abstract: A novel procedure has been developed to synthesize ordered carbon mesoporous carbons (OMC) containing well-dispersed and highly electrocatalytic Pt nanoparticles (Pt-OMC) for oxygen reduction reaction. Highlights: → A novel method to incorporate nanosized Pt particles on nanostructure carbons. → Functionalized silica templates were used to control size and distribution of Pt nanoparticles. → Electrochemical measurements of oxygen reduction demonstrated high catalytic activity compared to common commercial catalysts.

  7. Phosphorescent platinum(II) complexes bearing 2-vinylpyridine-type ligands: synthesis, electrochemical and photophysical properties, and tuning of electrophosphorescent behavior by main-group moieties.

    Science.gov (United States)

    Yang, Xiaolong; Xu, Xianbin; Zhao, Jiang; Dang, Jing-shuang; Huang, Zuan; Yan, Xiaogang; Zhou, Guijiang; Wang, Dongdong

    2014-12-15

    A series of 2-vinylpyridine-type platinum(II) complexes bearing different main-group blocks (B(Mes)2, SiPh3, GePh3, NPh2, POPh2, OPh, SPh, and SO2Ph, where Mes = 2-morpholinoethanesulfonic acid) were successfully prepared. As indicated by the X-ray single-crystal diffraction, the concerned phosphorescent platinum(II) complexes exhibit distinct molecular packing patterns in the solid state to bring forth different interactions between individual molecules. The photophysical characterizations showed that the emission maxima together with phosphorescent quantum yield of these complexes can also be affected by introducing distinct main-group moieties with electron-donating or electron-withdrawing characters. Furthermore, these 2-vinylpyridine-type platinum(II) complexes exhibit markedly different photophysical and electrochemical properties compared with their 2-phenylpyridine-type analogues, such as higher-lying highest occupied molecular orbital levels and lower-energy phosphorescent emissions. Importantly, these complexes can show good potential as deep red phosphorescent emitters to bring attractive electroluminescent performances with Commission Internationale de L'Eclairage (CIE) coordinates very close to the standard red CIE coordinates of (0.67, 0.33) recommended by the National Television Standards Committee. Hence, these results successfully established structure-property relationship concerning photophysics, electrochemistry, and electroluminescence, which will not only provide important information about the optoelectronic features of these novel complexes but also give valuable clues for developing novel platinum(II) phosphorescent complexes.

  8. Synthesis, structural characterization, electrochemical and biological studies on divalent metal chelates of a new ligand derived from pharmaceutical preservative, dehydroacetic acid, with 1,4-diaminobenzene

    Directory of Open Access Journals (Sweden)

    Sanaa M. Emam

    2017-05-01

    Full Text Available Cobalt(II, nickel(II, copper(II, zinc(II and cadmium(II complexes of new 3-acetyl-4-[(4-aminophenylamino]-6-methyl-2H-pyran-2-one (HL1 derived from dehydroacetic acid and 1,4-diaminobenzene were prepared and characterized. The structural features were determined from their elemental analyses, 1H, and 13C-NMR spectra, molar conductivities, magnetic moments, IR, UVvis. spectra, thermal analyses (D.T.A. and T.G.A. and E.S.R. measurements. Their magnetic susceptibility measurements and low conductance data provide evidence for the mono- or dimeric and non-electrolytic nature of the solid complexes. The E.S.R. spectra of copper(II complexes show axial type symmetry with covalent or ionic bond character. The electrochemical behavior of the complexes in DMF (dimethylformamide solvent at 298 K was studied. The biological activity of the ligand and its metal(II complexes was also studied. The obtained complexes showed higher activities than the free ligand in protecting the Egyptian cotton fields from Spodoptera littoralis larvae.

  9. Synthesis, characterization, single crystal X-ray determination, fluorescence and electrochemical studies of new dinuclear nickel(II) and oxovanadium(IV) complexes containing double Schiff base ligands.

    Science.gov (United States)

    Shafaatian, Bita; Ozbakzaei, Zahra; Notash, Behrouz; Rezvani, S Ahmad

    2015-04-05

    A series of new bimetallic complexes of nickel(II) and vanadium(IV) have been synthesized by the reaction of the new double bidentate Schiff base ligands with nickel acetate and vanadyl acetylacetonate in 1:1 M ratio. In nickel and also vanadyl complexes the ligands were coordinated to the metals via the imine N and enolic O atoms. The complexes have been found to possess 1:1 metals to ligands stoichiometry and the molar conductance data revealed that the metal complexes were non-electrolytes. The nickel and vanadyl complexes exhibited distorted square planar and square pyramidal coordination geometries, respectively. The emission spectra of the ligands and their complexes were studied in methanol. Electrochemical properties of the ligands and their metal complexes were also investigated in DMSO solvent at 150 mV s(-1) scan rate. The ligands and metal complexes showed both quasi-reversible and irreversible processes at this scan rate. The Schiff bases and their complexes have been characterized by FT-IR, 1H NMR, UV/Vis spectroscopies, elemental analysis and conductometry. The crystal structure of the nickel complex has been determined by single crystal X-ray diffraction. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Orientation-controlled synthesis and characterization of Bi{sub 2}Te{sub 3} nanofilms, and nanowires via electrochemical co-deposition

    Energy Technology Data Exchange (ETDEWEB)

    Erdogan, Ibrahim Y., E-mail: ibrahimyerdogan@gmail.co [Bingol University, Faculty of Sciences and Arts, Department of Chemistry, 12000 Bingol (Turkey); Demir, Umit [Atatuerk University, Faculty of Sciences, Department of Chemistry, 25240 Erzurum (Turkey)

    2011-02-01

    An electrochemical deposition technique based on co-deposition was used to deposit preferentially oriented Bi{sub 2}Te{sub 3} nanostructures (nanofilm, and nanowire). The shared underpotential deposition (UPD) potentials for both Bi and Te co-deposition were determined by cyclic voltammetric measurements. The scanning probe microscopy (scanning tunneling microscopy (STM) and atomic force microscopy (AFM)) and the X-ray diffraction (XRD) data indicated that the electrodeposition of Bi{sub 2}Te{sub 3} results in nanofilm-structured deposits with a preferential orientation at (0 1 5) and nanowired-structured deposits with a preferential orientation at (1 1 0) in acidic and basic (in the presence of ethylenediaminetetraacetic acid (EDTA)) medium, respectively. The results show that the nucleation and growth mechanism follows 3D mode in acidic solutions and 2D mode in basic solution containing EDTA additive. The optical characterization performed by reflection absorption Fourier transform infrared (RA-FTIR) spectroscopy showed that the band gap energy of Bi{sub 2}Te{sub 3} nanostructures depends on the thickness, size, and shape of the nanostructures and the band gap increases as the deposition time decreases. Moreover, the quantum confinement is strengthened in the wire-like deposits relative to the film-like deposits. Energy dispersive X-ray spectroscopy (EDS) analysis demonstrated that Bi{sub 2}Te{sub 3} nanostructures were always in 2:3 stoichiometry, and they were made up of only pure Bi and Te.

  11. Effect of reduction enhancer on a radiolytic synthesis of carbon-supported Pt–Cu nanoparticles and their structural and electrochemical properties

    Energy Technology Data Exchange (ETDEWEB)

    Kugai, Junichiro, E-mail: jkugai@kobe-kosen.ac.jp [Kobe City College of Technology, Department of Applied Chemistry (Japan); Kubota, Chihiro; Okazaki, Tomohisa; Seino, Satoshi; Nakagawa, Takashi [Osaka University, Graduate School of Engineering (Japan); Nitani, Hiroaki [High Energy Accelerator Research Organization, Institute of Materials Structure Science (IMSS) (Japan); Yamamoto, Takao A. [Osaka University, Graduate School of Engineering (Japan)

    2015-06-15

    In order to clarify the effect of reduction enhancer on the nanoparticle formation process and their structural and catalytic properties, carbon-supported Pt–Cu nanoparticles were synthesized by electron beam irradiation on an aqueous precursor solution in the presence/absence of reduction enhancer. In the absence of reduction enhancer, tetravalent platinum oxide particles of approximately 1 nm in diameter were formed on carbon support with copper barely precipitated, while in the presence of 2-propanol or ethylene glycol or glucose both platinum and copper precipitated as few-nanometer-sized alloy particles together with copper oxides. It was suggested that the metal nuclei produced upon electron beam irradiation do not have enough lifetime without reduction enhancer due to fast oxidation of the nuclei by oxidizing radicals, while the reduction enhancer scavenges these oxidizing radicals preventing oxidation of metallic clusters and prolonging their lifetime. Ethylene glycol gave smaller and better alloyed particles with less copper oxides compared to 2-propanol since the carbonyl compounds derived from oxidation of ethylene glycol protect metallic clusters from oxidation further prolonging their lifetime. In the electrochemical measurements, the methanol oxidation activities of Pt–Cu/C catalysts were well explained by their structural characteristics.

  12. Effect of reduction enhancer on a radiolytic synthesis of carbon-supported Pt-Cu nanoparticles and their structural and electrochemical properties

    Science.gov (United States)

    Kugai, Junichiro; Kubota, Chihiro; Okazaki, Tomohisa; Seino, Satoshi; Nakagawa, Takashi; Nitani, Hiroaki; Yamamoto, Takao A.

    2015-06-01

    In order to clarify the effect of reduction enhancer on the nanoparticle formation process and their structural and catalytic properties, carbon-supported Pt-Cu nanoparticles were synthesized by electron beam irradiation on an aqueous precursor solution in the presence/absence of reduction enhancer. In the absence of reduction enhancer, tetravalent platinum oxide particles of approximately 1 nm in diameter were formed on carbon support with copper barely precipitated, while in the presence of 2-propanol or ethylene glycol or glucose both platinum and copper precipitated as few-nanometer-sized alloy particles together with copper oxides. It was suggested that the metal nuclei produced upon electron beam irradiation do not have enough lifetime without reduction enhancer due to fast oxidation of the nuclei by oxidizing radicals, while the reduction enhancer scavenges these oxidizing radicals preventing oxidation of metallic clusters and prolonging their lifetime. Ethylene glycol gave smaller and better alloyed particles with less copper oxides compared to 2-propanol since the carbonyl compounds derived from oxidation of ethylene glycol protect metallic clusters from oxidation further prolonging their lifetime. In the electrochemical measurements, the methanol oxidation activities of Pt-Cu/C catalysts were well explained by their structural characteristics.

  13. Citrus maxima (Pomelo) juice mediated eco-friendly synthesis of ZnO nanoparticles: Applications to photocatalytic, electrochemical sensor and antibacterial activities

    Science.gov (United States)

    Pavithra, N. S.; Lingaraju, K.; Raghu, G. K.; Nagaraju, G.

    2017-10-01

    In the present work, Zinc oxide nanoparticles (ZnO Nps) have been successfully prepared through a simple, effective and low cost solution combustion method using Zn (NO3)2·6H2O as an oxidizer, chakkota (Common name = Pomelo) fruit juice as novel fuel. X-ray diffraction pattern indicates the hexagonal wurtzite structure with average crystallite size of 22 nm. ZnO Nps were characterized with the aid of different spectroscopic techniques such as Raman spectroscopy, Fourier Transform Infrared spectroscopy, Photoluminescence and UV-Visible spectroscopy. FTIR shows characteristic ZnO vibrational mode at 393 cm- 1. SEM images show that the particles are agglomerated. TEM image shows the size of the particles are about 10-20 nm. Further, in order to establish practical applicability of the synthesized ZnO Nps, photocatalytic degradation of methylene blue (MB) dye as a model system was studied in presence of UV (665 nm) light. In addition to this, the antibacterial activity was screen against 3 bacterial strains and electrochemical sensor performance towards the quantification of dopamine at nano molar concentrations was also explored.

  14. Hydrothermal synthesis of the clustered network-like Ni3S2-Co9S8 with enhanced electrochemical behavior for supercapacitor electrode

    Science.gov (United States)

    Han, Tao; Jiang, Liya; Jiu, Hongfang; Chang, Jianxia

    2017-11-01

    In this work, a facile one-pot solvothermal route has been employed in preparing the clustered network-like Ni3S2-Co9S8 on Ni foam substrate (Ni3S2-Co9S8/NF) worked as electrode of supercapacitor. Ni3S2-Co9S8/Ni foam obtained showed a high specific capacitance of 5.37 F cm2 at a current density of 5 mA cm2. Furthermore, an asymmetric supercapacitor has been assembled using Ni3S2-Co9S8/NF as positive electrode and activated carbon (AC) as negative electrode. The resulting Ni3S2-Co9S8/NF//AC device exhibited a high energy density of 17 Wh kg-1 at a power density of 1.4 kW kg-1 with good cycling performance (80% of the initial capacitance retention after 1000 cycles). The superior electrochemical performance can be attributed to the combined contribution of both component and unique clustered network-like. The results demonstrate that the Ni3S2-Co9S8/NF is promising as electrode material for supercapacitors in energy storage.

  15. Synthesis of Nano scale Heterostructures Comprised of Metal Nano wires, Carbon Nano tubes, and Metal Nanoparticles: Investigation of Their Structure and Electrochemical Properties

    International Nuclear Information System (INIS)

    Chopra, N.; Wu, J.; Chopra, N.; Agrawal, P.

    2014-01-01

    One-dimensional nano scale heterostructures comprised of multi segment gold-nickel nano wires, carbon nano tube, and nickel nanoparticles were fabricated in a unique approach combining top-down and bottom-up assembly methods. Porous alumina template was utilized for sequential electrodeposition of gold and nickel nano wire segments. This was followed by chemical vapor deposition growth of carbon nano tubes on multi segment gold-nickel nano wires, where nickel segment also acted as a carbon nano tube growth catalyst. The aligned arrays of these gold-nickel-carbon nano tube heterostructures were released from porous alumina template and then subjected to wet-chemical process to be decorated with nickel/nickel oxide core/shell nanoparticles. X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and Raman spectroscopy were utilized for morphology, interface, defect, and structure characterization. The electrochemical performance of these heterostructures was studied using cyclic voltammetry method and the specific capacitance of various heterostructures was estimated and compared.

  16. Synthesis of hollow silica nanosphere with high accessible surface area and their hybridization with carbon matrix for drastic enhancement of electrochemical property

    Science.gov (United States)

    Alam, Mohammad Mydul; Yamahana, Haruki; Bastakoti, Bishnu Prasad; Luitel, Hom Nath; Zhao, Wenwen; Yamauchi, Yusuke; Watari, Takanori; Noguchi, Hideyuki; Nakashima, Kenichi

    2014-09-01

    Hollow silica nanospheres with high accessible surface area have been synthesized by using core-shell-corona polymeric micelle of poly (styrene-b-2-vinyle pyridine-b-ethylene oxide) (PS45k-PVP26k-PEO82k) as a template. The size of the template polymeric micelle depends on the pH of the solution, i.e. ≈100 nm at pH 7 whereas ≈300 nm at pH 4. The enlarged size of the micelle is possibly due to the protonation of the PVP block, which also serves as reaction sites for silica precursor. The size of the obtained silica nanosphere measured with transmission electron microscope (TEM) is around ≈70 nm and shell thickness is ≈20 nm. Fourier transformed infrared spectroscopy (FTIR) data confirms that the polymer template is completely removed during calcination. Conductive carbon is doped into the silica nanosphere through glucose solution followed by hydrothermal treatment and pyrolysis. It is found that the electrochemical performance and stability of the silica nanosphere is dramatically enhanced after carbon doping. The combined strategy of the core-shell-corona micelle as template and carbon doping could represent a new platform for the researchers to develop functional nanomaterials.

  17. 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.

  18. Coordination-organometallic hybrid materials based on the trinuclear M(II)-Ru(II) (M=Ni and Zn) complexes: Synthesis, structural characterization, luminescence and electrochemical properties

    Science.gov (United States)

    Pawal, S. B.; Lolage, S. R.; Chavan, S. S.

    2018-02-01

    A new series of trinuclear complexes of the type Ni[R-C6H4Ndbnd CH(O)C6H3Ctbnd CRu(dppe)2Cl]2 (1a-c) and Zn[Rsbnd C6H4Ndbnd CH(O)C6H3Ctbnd CRu(dppe)2Cl]2 (2a-c) have been prepared from the reaction of trans-[RuCl(dppe)2Ctbnd Csbnd C6H3(OH)(CHO)] (1) with aniline, 4-nitroaniline and 4-methoxyaniline (R1-3) in presence of nickel acetate and zinc acetate in CH2Cl2/MeOH (1:1) mixture. The structural properties of the complexes have been characterized by elemental analyses and spectroscopic techniques viz. FTIR, UV-Visible, 1H NMR and 31P NMR spectral studies. The crystal structure and morphology of the hybrid complexes was investigated with the help of X-ray powder diffraction (XRPD), Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM). The thermal properties of 1a-c and 2a-c were studied by thermogravimetric (TG) analysis. The electrochemical behaviour of the complexes reveals that all complexes displayed a quasireversible redox behaviour corresponding to Ru(II)/Ru(III) and Ni(II)/Ni(III) couples for 1a-c and only Ru(II)/Ru(III) couple for 2a-c. All complexes are emissive in solution at room temperature revealing the influence of substituents and solvent polarity on emission properties of the complexes.

  19. Synthesis and electrochemical performance of mesoporous SiO{sub 2}–carbon nanofibers composite as anode materials for lithium secondary batteries

    Energy Technology Data Exchange (ETDEWEB)

    Hyun, Yura; Choi, Jin-Yeong [Department of Chemistry, Keimyung University (Korea, Republic of); Park, Heai-Ku [Department of Chemical Engineering, Keimyung University (Korea, Republic of); Bae, Jae Young [Department of Chemistry, Keimyung University (Korea, Republic of); Lee, Chang-Seop, E-mail: surfkm@kmu.ac.kr [Department of Chemistry, Keimyung University (Korea, Republic of)

    2016-10-15

    Highlights: • Mesoporous SiO{sub 2}–carbon nanofibers composite synthesized on Ni foam without any binder. • This composite was directly applied as anode material of Li secondary batteries. • Showed the highest initial (2420 mAh/g) and discharging (2092 mAh/g) capacity. • This material achieved a retention rate of 86.4% after 30 cycles. - Abstract: In this study, carbon nanofibers (CNFs) and mesoporous SiO{sub 2}–carbon nanofibers composite were synthesized and applied as the anode materials in lithium secondary batteries. CNFs and mesoporous SiO{sub 2}–CNFs composite were grown via chemical vapor deposition method with iron-copper catalysts. Mesoporous SiO{sub 2} materials were prepared by sol–gel method using tetraethylorthosilicate as the silica source and cetyltrimethylammoniumchloride as the template. Ethylene was used as the carbon source and passes into a quartz reactor of a tube furnace heated to 600 °C, and the temperature was maintained at 600 °C for 10 min to synthesize CNFs and mesoporous SiO{sub 2}–CNFs composite. The electrochemical characteristics of the as-prepared CNFs and mesoporous SiO{sub 2}–CNFs composite as the anode of lithium secondary batteries were investigated using a three-electrode cell. In particular, the mesoporous SiO{sub 2}–CNFs composites synthesized without binder after depositing mesoporous SiO{sub 2} on Ni foam showed the highest charging and discharging capacity and retention rate. The initial capacity (2420 mAh/g) of mesoporous SiO{sub 2}–CNFs composites decreased to 2092 mAh/g after 30 cycles at a retention rate of 86.4%.

  20. 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.

  1. Electrochemical catalysis of styrene epoxidation with films of manganese dioxide nanoparticles, and, Synthesis of mixed metal oxides using ultrasonic nozzle spray and microwaves

    Science.gov (United States)

    Espinal, Laura

    Films of polyions and octahedral layered manganese oxide (OL-1) nanoparticles on carbon electrodes made by layer-by-layer alternate electrostatic adsorption were active for electrochemical catalysis of styrene epoxidation in solution in the presence of hydrogen peroxide and oxygen. The highest catalytic turnover was obtained by using applied voltage -0.6 V vs. SCE, O2, and 100 mM H2O2. 18O isotope labeling experiments suggested oxygen incorporation from three different sources: molecular oxygen, hydrogen peroxide and/or lattice oxygen from OL-1 depending on the potential applied and the oxygen and hydrogen peroxide concentrations. Oxygen and hydrogen peroxide activate the OL-1 catalyst for the epoxidation. The pathway for styrene epoxidation in the highest yields required oxygen, hydrogen peroxide and a reducing voltage, and may involve an activated oxygen species in the OL-1 matrix. Multicomponent metal oxide (MMO) crystallites were prepared by spraying a reactant solution into a receiving solution or air under microwave radiation at atmospheric pressure. The injection of nitric acid solution through an ultrasonic nozzle into a receiving solution of metal precursor and the use of microwave radiation were combined to form a novel preparation technique called the nozzle-spray/microwave (NMW) method. The inclusion of an additional step, the in situ mixing of precursor solutions prior to their injection through the ultrasonic nozzle spray, led to another procedure called the in situ/nozzle-spray/microwave (INM) method. For comparison, MMO materials with the same metal constituents as those prepared by our novel techniques were prepared by conventional hydrothermal (CH) methods. Fresh materials prepared by NMW, INM and CH methods were heat treated to study the effect of calcination. All materials were characterized before and after calcination using XRD, SEM, Bet, and ICP. The NMW method produces particles with rod-like morphologies different from those obtained using

  2. Synthesis and evaluation of MoWCoS/G and MoWCuS/G as new transition metal dichalcogenide nanocatalysts for electrochemical hydrogen evolution reaction

    Science.gov (United States)

    Askari, Mohammad Bagher; Beheshti-Marnani, Amirkhosro; Banizi, Zoha Tavakoli; Seifi, Majid; Ramezan zadeh, Mohammad Hassan

    2018-01-01

    New nanocomposites based on transition metal dichalcogenides, MoWCoS and MoWCuS, were synthesized through one step hydrothermal method. X-ray diffraction (XRD) and energy dispersive X-ray (EDX) techniques as well as field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) images confirmed the synthesis of nanocomposites. For investigation of hydrogen evolution reaction (HER) properties of new nanocomposites, linear sweep voltammetry (LSV) was applied for this purpose. According to the results of similar previous works, the prepared nanocomposites showed promising HER properties as low overpotential equal to 41.4 mV/dec for MoWCoS hybridized with reduced graphene (G) and a little higher one equal to 49 mV/dec for MoWCuS hybridized with reduced graphene. Based on obtained Tafel slopes 38 and 53 mV/dec for MoWCoS/G and MoWCuS/G, respectively, the "Heyrovsky-Volmer" mechanism was suggested for the new HER three component nanocatalysts as the first effort to this purpose.

  3. Green and facile synthesis of an Au nanoparticles@polyoxometalate/ordered mesoporous carbon tri-component nanocomposite and its electrochemical applications.

    Science.gov (United States)

    Zhang, Yufan; Bo, Xiangjie; Nsabimana, Anaclet; Munyentwali, Alexis; Han, Ce; Li, Mian; Guo, Liping

    2015-04-15

    The one-pot synthesis of a well-defined Au nanoparticles@polyoxometalates/ordered mesoporous carbon (Au@POMs/OMC) tri-component nanocomposite is reported, which is facile, green and rapid. The polyoxometalates were used as both reductant and bridging molecules. The formation of these composite materials was verified by a comprehensive characterization using X-ray diffraction, X-ray photoelectron spectroscopy, energy-dispersive X-ray spectra, scanning electron microscopy, and transmission electron microscopy. The novel nanohybrids of Au@POMs/OMC can provide new features of electrocatalytic activities, because of the synergetic effects of Au nanoparticles and OMC materials. Most importantly, the amperometric measurements show that the Au@POMs/OMC nanohybrids have a high catalytic activity with a good sensitivity, long-term stability, wide linear range, low detection limit, and fast response towards acetaminophenol, H2O2, and NADH detection for application as an enzyme-free biosensor. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Synthesis and electrochemical properties of KPb{sub 4−x}Ca{sub x}(PO{sub 4}){sub 3} (0 ≤ x ≤ 1.5) for oxidation of cadmium at graphite electrode

    Energy Technology Data Exchange (ETDEWEB)

    Lahrich, Sara [Univ Hassan 1, Laboratoire de Chimie et Modélisation Mathématique, Faculté Polydisciplinaire, 25000 Khouribga (Morocco); Univ Hassan 1, Laboratoire Sciences des Matériaux, des Milieux et de la Modélisation, Faculté Polydisciplinaire, 25000 Khouribga (Morocco); Manoun, Bouchaib [Univ Hassan 1, Laboratoire Sciences des Matériaux, des Milieux et de la Modélisation, Faculté Polydisciplinaire, 25000 Khouribga (Morocco); El Mhammedi, Moulay Abderrahim, E-mail: elmhammedi@yahoo.fr [Univ Hassan 1, Laboratoire de Chimie et Modélisation Mathématique, Faculté Polydisciplinaire, 25000 Khouribga (Morocco)

    2017-02-15

    Chemically modified carbon paste electrode (CPE) for cadmium (II) analysis has been constructed by mixing KPb{sub 4−x}Ca{sub x}(PO{sub 4}){sub 3} (0 ≤ x ≤ 1.5) (CaLA) and graphite powder. The lacunar apatite was synthesized using solid reaction and characterized by X-ray diffraction (XRD), infrared spectroscopy (IR) and Raman spectroscopy. The refinement study was carried out using Rietveld method where the obtained results show a good agreement between the observed and calculated patterns. The detection of cadmium (II) was investigated in acetate buffer (pH 4.5) using differential pulse anodic stripping voltammetry (DPASV). The limit of detection obtained under the optimized experimental conditions was 5.35 × 10{sup −7} mol L{sup −1} with a relative standard deviation of 2.37%. Possible interferences were tested and evaluated in 5.0 × 10{sup −5} mol L{sup −1} cadmium (II) in the presence of other inorganic ions. Finally, the proposed method was successfully applied to determine cadmium (II) in seawater and mussel samples. Hence, the satisfactory results confirm the applicability of this sensor in practical analysis. - Highlights: • Synthesis and characterization of new lacunar apatites KPb{sub 4−x}Ca{sub x}(PO{sub 4}){sub 3} (0 ≤ x ≤ 1.5). • Structural refinement of these compounds using Rietveld method. • A study of Ca doping effect in lacunar apatites for detecting Cd (II). • The electrochemical oxidation of Cd (II) was performed at CaLA-CPE using DPASV. • The proposed method was evaluated to detect cadmium in seawater and mussel samples.

  5. Synthesis of novel monomeric graphene quantum dots and corresponding nanocomposite with molecularly imprinted polymer for electrochemical detection of an anticancerous ifosfamide drug.

    Science.gov (United States)

    Bali Prasad, Bhim; Kumar, Anil; Singh, Ragini

    2017-08-15

    This paper reports a typical synthesis of a nanocomposite of functionalized graphene quantum dots and imprinted polymer at the surface of screen-printed carbon electrode using N-acryloyl-4-aminobenzamide, as a functional monomer, and an anticancerous drug, ifosfamide, as a print molecule (test analyte). Herein, graphene quantum dots in nanocomposite practically induced the electrocatalytic activity by lowering the oxidation overpotential of test analyte and thereby amplifying electronic transmission, without any interfacial barrier in between the film and the electrode surface. The differential pulse anodic stripping signal at functionalized graphene quantum dots based imprinted sensor was realized to be about 3- and 7-fold higher as compared to the traditionally made imprinted polymers prepared in the presence and the absence of graphene quantum dots (un-functionalized), respectively. This may be attributed to a pertinent synergism in between the positively charged functionalized graphene quantum dots in the film and the target analyte toward the enhancement of electro-conductivity of the film and thereby the electrode kinetics. In fact, the covalent attachment of graphene quantum dots with N-acryloyl-4-aminobenzamide molecules might exert an extended conjugation at their interface facilitating electro conducting to render the channelized pathways for the electron transport. The proposed sensor is practically applicable to the ultratrace evaluation of ifosfamide in real (biological/pharmaceutical) samples with detection limit as low as 0.11ngmL -1 (S/N=3), without any matrix effect, cross-reactivity, and false-positives. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. 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.

  7. 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.

  8. Synthesis of IV-VI Transition Metal Carbide and Nitride Nanoparticles Using a Reactive Mesoporous Template for Electrochemical Hydrogen Evolution Reaction

    KAUST Repository

    Alhajri, Nawal Saad

    2016-01-01

    content rather than nitride. In addition, the reactivity of the transition metals of group IV-VI with the reactive template was investigated under a flow of N2 at different temperatures in the range of 1023 to 1573 K while keeping the weight ratio constant at 1:1. The results show that Ti, V, Nb, Ta, and Cr reacted with mpg-C3N4 at 1023 K to form nitride phase with face centered cubic structure. The nitride phase destabilized at higher temperature ≥1223 K through the reaction with the remaining carbon residue originated from the decomposition of the template to form carbonitride and carbide phases. Whereas, Mo and W produce a hexagonal structure of carbide irrespective of the applying reaction temperature. The tendency to form transition metal nitrides and carbides at 1023 K was strongly driven by the free energy of formation. The observed trend indicates that the free energy of formation of nitride is relatively lower for group IV and V transition metals, whereas the carbide phase is thermodynamically more favorable for group VI, in particular for Mo and W. The thermal stability of nitride decreases at high temperature due to the evolution of nitrogen gas. The electrocatalytic activities of the produced nanoparticles were tested for hydrogen evolution reaction in acid media and the results demonstrated that molybdenum carbide nanoparticles exhibited the highest HER current with over potential of 100 mV vs. RHE, among the samples prepared in this study. This result is attributed to the sufficiently small particle size (8 nm on average) and accordingly high surface area (308 m2 g-1). Also, the graphitized carbon layer with a thickness of 1 nm on its surface formed by this synthesis provides excellent electron pathway to the catalyst which will improve the rate of electron transfer reaction.

  9. Synthesis and electrochemical performance of Sn-doped Li3V2(PO4)3/C cathode material for lithium ion battery by microwave solid-state technique

    International Nuclear Information System (INIS)

    Liu, Haiping; Bi, Sifu; Wen, Guangwu; Teng, Xiangguo; Gao, Peng; Ni, Zujun; Zhu, Yongming; Zhang, Fang

    2012-01-01

    Highlights: ► Li 3 V 2−x Sn x (PO 4 ) 3 /C (0 ⩽ x ⩽ 0.10) cathode is first reported. ► Sn doping improves the initial discharge capacity and the cycle stability of Li 3 V 2 (PO 4 ) 3 /C. ► Sn doping improves the conductivity and reversibility of the Li 3 V 2 (PO 4 ) 3 /C. - Abstract: Li 3 V 2−x Sn x (PO 4 ) 3 /C cathode materials with uniform and fine particle sizes were successfully and fast synthesized by a microwave solid-state synthesis method. X-ray diffraction patterns demonstrated that the appropriate addition of Sn did not destroy the lattice structure of Li 3 V 2 (PO 4 ) 3 /C, but decreased the unit cell volume. X-ray photoelectron spectroscopy analysis demonstrated that the main chemical state of V in the Li 3 V 1.95 Sn 0.05 (PO 4 ) 3 /C composite is +3 valence, while the chemical state of Sn in the Li 3 V 1.95 Sn 0.05 (PO 4 ) 3 /C is +4 valence. Scanning electron microscope analysis illustrated that the addition of Sn slightly affected the morphology of samples. As the cathode materials for Li-ion batteries, Li 3 V 2−x Sn x (PO 4 ) 3 /C (x ⩽ 0.10) exhibited higher discharge capacity and better cycle stability than the pure one. At a discharge rate of 0.5 C in the potential range of 2.5–4.5 V at room temperature, the initial discharge capacity of Li 3 V 1.95 Sn 0.05 (PO 4 ) 3 /C was 136 mA h/g. The low charge-transfer resistances and large lithium ion diffusion coefficients confirmed that Sn-doped Li 3 V 2 (PO 4 ) 3 /C samples possessed better electronic conductivity and lithium ion mobility. These improved electrochemical performances can be attributed to the appropriate amount of Sn doping in Li 3 V 2 (PO 4 ) 3 /C system by enhancing structural stability and electrical conductivity. The present study also demonstrates that the microwave processing is a fast, simple and useful method for the fabrication of Li 3 V 2 (PO 4 ) 3 /C crystals.

  10. 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.

  11. Electrochemical Analysis of Neurotransmitters

    Science.gov (United States)

    Bucher, Elizabeth S.; Wightman, R. Mark

    2016-01-01

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

  12. Electrochemical Sensors: Functionalized Silica

    Energy Technology Data Exchange (ETDEWEB)

    Fryxell, Glen E.; Lin, Yuehe; Yantasee, Wassana

    2009-03-24

    This chapter summarizes recent devellopment of electrochemical sensors based on functionlized mesoporous silica materials. The nanomatrials based sensors have been developed for sensitive and selective enrironmental detection of toxic heavy metal and uranium ions.

  13. 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.

  14. Fundamentals of electrochemical science

    CERN Document Server

    Oldham, Keith

    1993-01-01

    Key Features* Deals comprehensively with the basic science of electrochemistry* Treats electrochemistry as a discipline in its own right and not as a branch of physical or analytical chemistry* Provides a thorough and quantitative description of electrochemical fundamentals

  15. Electrochemical and optical properties of a new donor–acceptor ...

    Indian Academy of Sciences (India)

    Abstract. In this communication, we report the synthesis and characterization of a new donor–acceptor type conjugated polymer carrying alternate 3 ..... Figure 3. TGA trace of the polymer P1. Table 1. Electrochemical potentials, energy levels and energy barriers for electron/hole injection for the polymer P1. Polymer. Eons.

  16. Electrochemical sensing and photocatalysis using Ag-TiO 2 ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 124; Issue 5. Electrochemical ... Anatase Ag-TiO2 microwires with high sensitivity and photocatalytic activity were synthesized via polyol synthesis route followed by a simple surface modification and chemical reduction approach for attachment of silver. The superior ...

  17. Solid state electrochemical composite

    Science.gov (United States)

    Visco, Steven J.; Jacobson, Craig P.; DeJonghe, Lutgard C.

    2009-06-30

    Provided is a composite electrochemical device fabricated from highly electronically conductive materials such as metals, metal alloys, or electronically conductive ceramics. The electronic conductivity of the electrode substrate is maximized. The invention allows for an electrode with high electronic conductivity and sufficient catalytic activity to achieve high power density in ionic (electrochemical) devices such as fuel cells and electrolytic gas separation systems including oxygen generation system.

  18. Electrochemical synthesis and characterization of polyconjugated polyfuran

    Energy Technology Data Exchange (ETDEWEB)

    Zotti, G.; Schlavon, G.; Comisso, N. (Consiglio Nazionale delle Ricerche, Ist. di Polarografia ed Elettrochimica Preparativa, Padua (Italy)); Berlin, A.; Pagani, G. (Dipt. di Chimica Organica e Industriale, Milan Univ. (Italy) Centro CNR, Speciali Sistemi Organici, Milan (Italy))

    1990-07-01

    Polyconjugated polyfuran (PF) was produced by electroreduction of 2,5-dibromofuran in acetonitrile using Ni(bipy){sub 3}{sup 2+} as catalyst. Polymerization occurs only in the presence of excess Ni(bipy){sub 3}{sup 2+} at potentials in the range -1.7 to -2.0 V versus Ag/Ag{sup +} via binuclear organonickel complex. IR spectroscopy, elemental analysis and mass spectroscopy confirm that PF is constituted by 2.5-linked furan units and indicate a degree of polymerization >100. Red PF films ({lambda}{sub max}=420 nm, E{sub g}=2.2 eV) are reversibly oxidized at 0.45 V and reduced at -2.5 V.Doping with AsF{sub 5} gives PF a conductivity of 10{sup -3} S/cm. Polymers produced by anodic coupling of furan were also investigated for comparison. IR spectroscopy and elemental analysis indicate that they display a lower degree of conjugation due to the concomitant acidcatalyzed polymerization. (orig.).

  19. Synthesis, characterization and electrochemical performance of ...

    Indian Academy of Sciences (India)

    Introduction. The rechargeable lithium ion batteries for portable electronic devices (e.g., PC and laptop computers, wireless and mobile phones, camcorders, etc.) .... Galvanostatic charging and discharging cyclings of the cells were achieved with the potentials windows between 1.5 and. 4.5 V at total current 0.1 mA using a ...

  20. Synthesis and electrochemical studies of phenylazo substituted ...

    Indian Academy of Sciences (India)

    Unknown

    The controlled potential electrolysis was carried out at –0⋅63 V for the nitro compound. After sometime, the samples of the cathodic solution were removed, diluted to a fixed volume with DMF and spectral examinations were made. It was found that there is a decrease in the peak at 518 nm due to the dye, with increasing ...

  1. Synthesis, optical and electrochemical characterization of ...

    African Journals Online (AJOL)

    ... photoluminescence efficiency while polymer P2 does not show any significant light emission up to 8.0 V. The results show the need for balance of electron and hole transport in polymer light emitting diodes. KEY WORDS: Anthracene, Benzothiadiazole, Polyfluorene copolymers, Photoluminescence, Light emitting diode.

  2. Electrochemical synthesis and characterization of chloride doped ...

    Indian Academy of Sciences (India)

    Unknown

    1. Introduction. Research in electroactive polymers, particularly in aromatic conducting polymers, has received considerable attention worldwide in the past few years because of their potential applications in the fields of microelectronics, optics and optoelectronics (Bernard et al 1998, 2001;. Schultze et al 1999; Mousty et al ...

  3. Synthesis, Photophysical, Electrochemical and Thermal Studies of ...

    Indian Academy of Sciences (India)

    with Tetramethylsilane (TMS) as internal reference at a working frequency of 300 MHz and 75 MHz respec- tively. Fourier transform infrared (FT–IR) spectra were ... interface using GPES software version 4.9.005. Typically, a three electrode cell equipped with a glassy carbon working electrode, Ag/AgCl (non-aqueous).

  4. Hydrothermal synthesis and electrochemical properties of a ...

    Indian Academy of Sciences (India)

    Coordination polymers are a new generation of solid- state materials that have promising applications in gas storage, catalysis, and porous materials due to their unique structural and functional properties.7–9 In virtue of their special properties, it is appealing to construct. POM-based coordination polymers, which may com-.

  5. Controlled synthesis and electrochemical properties of vanadium ...

    Indian Academy of Sciences (India)

    Administrator

    . Those compounds probably contained vanadium atoms in +4 oxidation state as con- firmed by a previous study (Livage 1998). TEM image. (figure S4a) of the sample obtained at 120°C revealed that it consisted of a number of nanosheets, ...

  6. electrochemical synthesis and spectroscopic characterization of poly ...

    African Journals Online (AJOL)

    a

    on Pt and Fe electrodes in an aqueous micellar medium containing sodium dodecylsulfate and. 10-3 M bithiophene (BT) ... phenylpyrrole) electrosynthesized on Pt, in organic and micellar media. However, to the .... the iron oxides and/or hydroxides formed because of the presence of residual amounts of water in acetonitrile ...

  7. Synthesis, photophysical, electrochemical and thermal investigation ...

    Indian Academy of Sciences (India)

    field effect transistors (OFETs)2 and dye-sensitized solar cells.3 Since the .... toluene, chloroform, acetonitrile etc. However, they are sparingly soluble in alcohols and insoluble in water. 2.2a 2,7–Dibromoxanthen–9–one (1): Bromination of xanthone was ..... On anodic sweeps, no oxidation wave was observed for the parent ...

  8. Controlled synthesis and electrochemical properties of vanadium ...

    Indian Academy of Sciences (India)

    Administrator

    oxides with different nanostructures by Yifu Zhang et al (pp 369–376). The composition and vanadium valence state of the surface of typical V3O7·H2O and VO2(B) nanobelts were investigated by XPS test, as shown in figure S1. The survey spectra (figures S1a and S1c) reveal that both. V3O7·H2O and VO2(B) only consist ...

  9. Synthesis, Spectral, Electrochemical and Theoretical Investigation of ...

    Indian Academy of Sciences (India)

    Their absorption and photoluminescence properties were investigated in various solvents and in neat solid film and found to possess characteristic electronic absorption and emission spectra which stronglydepend on the nature of solvents used. Compounds show intramolecular charge transfer transitions (ICT) in the range ...

  10. Synthesis, photophysical, electrochemical and thermal investigation ...

    Indian Academy of Sciences (India)

    Organic semiconductors have received considerable attention during the last few decades because of funda- mental curiosity about their electro-optical properties and technological applications. Organic π–conjugated molecules have been explored for their application as organic light emitting diodes (OLEDs),1 organic.

  11. Synthesis, Photophysical, Electrochemical and Thermal Studies of ...

    Indian Academy of Sciences (India)

    charge transfer (ICT) excited states13,14 or sometimes even from intermolecular excimers or exciplexes.15,16. Thus, appropriate selection of the donor–acceptor units allows us to control photoluminescence prop- erties, HOMO-LUMO energy levels and bandgap of the D-A molecules. Many donor-acceptor molecules.

  12. Synthesis, spectroscopic, electrochemical and luminescence studies ...

    Indian Academy of Sciences (India)

    Unknown

    with hydrazine to form its N2 complex which is of great interest in the chemistry of N2 fixation. Triazoles are also the subject of extensive studies in view of their synthetic properties and other theoretical aspects 9. Ruthenium (II) polypyridyl complexes have opened a new door for enthusiastic researchers since they act as ...

  13. Synthesis, spectroscopic, electrochemical and luminescence studies ...

    Indian Academy of Sciences (India)

    Unknown

    Substituted 1,2,4-triazoles have attracted attention owing to their bactericidal 1, fungicidal 2 and pharmacological activities 3,4 in addition to their uses as antiulcer 5 and blood-pressure-lowering agents 6. Furthermore, it is known 7,8 that RuCl3.3H2O reacts with hydrazine to form its N2 complex which is of great interest in ...

  14. 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 by a facile hydrothermal approach using glucose as the reducing and structure-directing reagent. The as-obtained V3O7.H2O nanobelts have a length up to several tens of micrometers, width of about 60–150 nm and ...

  15. Synthesis, characterization and electrochemical performance of ...

    Indian Academy of Sciences (India)

    2017-09-06

    Sep 6, 2017 ... at 0.1C rate. The cycle life performance of all Li2Nix Fe1−x SiO4 batteries ranged between 100 and 156 mAh g. −1 with coulombic efficiency range between 70.9 and. 93.9%. Keywords. ... cathode materials suffer from the high to low rate capability due to its ..... The exchange current density is i = RT/nFRct).

  16. Electrochemical synthesis and spectroscopic characterization of ...

    African Journals Online (AJOL)

    phenylpyrrole) coatings in an organic medium on iron and platinum electrodes. ... XPS measurements, infrared (FT-IR) and electronic absorption (UV-vis) spectroscopies were used to characterize the iron and platinum-coated electrodes. Finally the ...

  17. Cu-based materials as high-performance electrodes toward electrochemical energy storage

    Science.gov (United States)

    Chen, Kunfeng; Xue, Dongfeng

    2014-02-01

    Cu-based materials, including metal Cu and semiconductors of Cu2O and CuO, are promising and important candidates toward practical electrochemical energy storage devices due to their abundant, low cost, easy synthesis and environmentally friendly merits. This review presents an overview of the applications of Cu-based materials in the state-of-art electrochemical energy storage, including both lithium-ion batteries and supercapacitors. The synthesis chemistry, structures and the corresponding electrochemical performances of these materials are summarized and compared. During chemical synthesis and electroactive performance measurement of Cu-based materials, we found that Cu-Cu2O-CuO sequence governs all related transformations. Novel water-soluble CuCl2 supercapacitors with ultrahigh capacitance were also reviewed which can advance the understanding of intrinsic mechanism of inorganic pseudocapacitors. The major goal of this review is to highlight some recent progresses in using Cu-based materials for electrochemical energy storage.

  18. Graphene directed architecture of fine engineered nanostructures with electrochemical applications

    DEFF Research Database (Denmark)

    Hou, Chengyi; Zhang, Minwei; Halder, Arnab

    2017-01-01

    . 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...... 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...... and future perspective in the graphene-templating design and synthesis of various materials. Overall, this review could offer crucial insights into the nanoscale engineering of new nanostructures using graphene as a soft template and their potential applications in electrochemical science and technology. We...

  19. Azapeptide Synthesis Methods for Expanding Side-Chain Diversity for Biomedical Applications.

    Science.gov (United States)

    Chingle, Ramesh; Proulx, Caroline; Lubell, William D

    2017-07-18

    Mimicry of bioactive conformations is critical for peptide-based medicinal chemistry because such peptidomimetics may augment stability, enhance affinity, and increase specificity. Azapeptides are peptidomimetics in which the α-carbon(s) of one or more amino acid residues are substituted by nitrogen. The resulting semicarbazide analogues have been shown to reinforce β-turn conformation through the combination of lone pair-lone pair repulsion of the adjacent hydrazine nitrogen and urea planarity. Substitution of a semicarbazide for an amino amide residue in a peptide may retain biological activity and add benefits such as improved metabolic stability. The applications of azapeptides include receptor ligands, enzyme inhibitors, prodrugs, probes, and imaging agents. Moreover, azapeptides have proven therapeutic utility. For example, the aza-glycinamide analogue of the luteinizing hormone-releasing hormone analogue Zoladex is a potent long-acting agonist currently used in the clinic for the treatment of prostate and breast cancer. However, the use of azapeptides was hampered by tedious solution-phase synthetic routes for selective hydrazine functionalization. A remarkable stride to overcome this bottleneck was made in 2009 through the introduction of the submonomer procedure for azapeptide synthesis, which enabled addition of diverse side chains onto a common semicarbazone intermediate, providing a means to construct azapeptide libraries by solution- and solid-phase chemistry. In brief, aza residues are introduced into the peptide chain using the submonomer strategy by semicarbazone incorporation, deprotonation, N-alkylation, and orthogonal deprotection. Amino acylation of the resulting semicarbazide and elongation gives the desired azapeptide. Since the initial report, a number of chemical transformations have taken advantage of the orthogonal chemistry of semicarbazone residues (e.g., Michael additions and N-arylations). In addition, libraries have been synthesized

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

    Science.gov (United States)

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

    2018-03-01

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

  1. Electrochemical energy storage

    CERN Document Server

    Tarascon, Jean-Marie

    2015-01-01

    The electrochemical storage of energy has become essential in assisting the development of electrical transport and use of renewable energies. French researchers have played a key role in this domain but Asia is currently the market leader. Not wanting to see history repeat itself, France created the research network on electrochemical energy storage (RS2E) in 2011. This book discusses the launch of RS2E, its stakeholders, objectives, and integrated structure that assures a continuum between basic research, technological research and industries. Here, the authors will cover the technological

  2. Ionic liquids, method for the production thereof, and use of same as electrolytes for electrochemical energy storage devices

    OpenAIRE

    Miguel, Irene de; Herradón García, Bernardo; Mann, Enrique; Morales, Enrique

    2014-01-01

    [EN] The invention relates to ionic liquids of general formula (I), to the synthesis thereof, and to the use of said ionic liquids as electrolytes in electrochemical electrical energy storage devices.

  3. Electrochemical nitridation of metal surfaces

    Science.gov (United States)

    Wang, Heli; Turner, John A.

    2015-06-30

    Electrochemical nitridation of metals and the produced metals are disclosed. An exemplary method of electrochemical nitridation of metals comprises providing an electrochemical solution at low temperature. The method also comprises providing a three-electrode potentiostat system. The method also comprises stabilizing the three-electrode potentiostat system at open circuit potential. The method also comprises applying a cathodic potential to a metal.

  4. SPECTROPHOTOMETRIC AND ELECTROCHEMICAL STUDIES ...

    African Journals Online (AJOL)

    ABSTRACT. Spectrophotometric and electrochemical studies concerning the interaction of cryptand 222 with DDQ and I2 have been performed in ethanol solution. In the case of DDQ, the results are indicative of the formation of C222+ and DDQ- through an equilibrium reaction. The results of I2 indicate the formation of ...

  5. ELECTROCHEMICAL BEHAVIOUR AND VOLTAMMETRIC ...

    African Journals Online (AJOL)

    The electrochemical behaviour of Geshoidin was investigated at a glassy carbon electrode in mixtures of citric acid and di-sodium hydrogen orthophosphate aqueous buffer system over a wide pH range (pH 2-11) using cyclic voltammetry. Chemically irreversible single oxidation and reduction peaks were obtained in the ...

  6. Electrochemical Power Sources

    Indian Academy of Sciences (India)

    Home; Journals; Resonance – Journal of Science Education; Volume 6; Issue 7. Electrochemical Power Sources - Rechargeable Batteries. A K Shukla S K Martha. General Article Volume 6 Issue 7 July 2001 pp 52-63. Fulltext. Click here to view fulltext PDF. Permanent link:

  7. Synthesis, electrochemical investigation and EPR spectroscopy of a reversible four-stage redox system based on mesoionic 5,5'-azinobis(1,3-diphenyltetrazole) and related mesoionic compounds

    OpenAIRE

    Shuki, Araki; Kaori, Yamamoto; Tomoko, Inoue; Koji, Fujimoto; Hatsuo, Yamamura; Masao, Kawai; Yasuo, Butsugan; Jinkui, Zhou; Emerich, Eichhorn; Anton, Rieker; Martina, Huber

    1999-01-01

    Mesoionic 5,5′-azinobis(1,3-diphenyltetrazole) 1 was prepared, and its chemical oxidation gave stable crystals of the corresponding radical cation 1?+ and dication 12+, which reversibly gave back azine 1 on reduction with zinc. Electrochemical investigations of 1 using cyclovoltammetry and differential pulse voltammetry in pyridine (Py) or dichloromethane (DCM) also revealed the two reversible successive one-electron oxidations leading to dication 12+via radical cation 1?+, both of which can ...

  8. Recent Advances on Porous Carbon Materials for Electrochemical Energy Storage.

    Science.gov (United States)

    Wang, Libin; Hu, Xianluo

    2018-04-17

    The climate change and energy crisis promote the rapid development of electrochemical energy-storage devices. Of many intriguing physicochemical properties such as excellent chemical stability, high electronic conductivity and large specific surface area, porous carbon materials have always been considering as a promising candidate for electrochemical energy storage. Up to date, a wide variety of porous carbon materials upon molecular design, pore control and compositional tailoring have been proposed for energy-storage applications. This focus review summaries recent advances in the synthesis of various porous carbon materials from the view of energy storage, especially in the past three years. Their applications in representative electrochemical energy storage devices like lithium-ion batteries, supercapacitors, lithium-ion hybrid capacitors have been discussed in this review, looking forward to offering some inspirations and guidelines for the exploitation of advanced carbon-based energy-storage materials. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Electrochemical Hydrogen Evolution

    DEFF Research Database (Denmark)

    Laursen, A.B.; Varela Gasque, Ana Sofia; Dionigi, F.

    2012-01-01

    The electrochemical hydrogen evolution reaction (HER) is growing in significance as society begins to rely more on renewable energy sources such as wind and solar power. Thus, research on designing new, inexpensive, and abundant HER catalysts is important. Here, we describe how a simple experiment....... This exercise circumvents the complexity of traditional experiments while it still demonstrates the trends of the HER volcano known from literature....

  10. Electrochemical flow capacitors

    Science.gov (United States)

    Gogotsi, Yury; Presser, Volker; Kumbur, Emin Caglan

    2015-10-27

    The present invention generally relates to devices for energy storage technologies, and more particularly to electrochemical flow capacitor systems and applications. In some aspects, these flow capacitors have at least one electrode comprising a non-stationary solid or semi-solid composition comprising supercapacitive particles and an electrolytic solvent in electrical communication with at least one current collector, and energy is stored and/or released by charging and/or discharging the electrode(s).

  11. 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...

  12. Electrochemical C-O Bond Formation: A Facile Access to Aromatic Lactones.

    Science.gov (United States)

    Dai, Jian-Jun; Tao, Xiang-Zhang; Zhou, Jie; Xu, Jun; Xu, Hua-Jian

    2018-03-07

    An efficient and robust methodology based on electrochemical techniques for the direct synthesis of aromatic lactones via dehydrogenative C-O cyclization is described. This new and useful electrochemical reaction can tolerate a variety of functional groups, and is scalable to 100 grams under mild conditions. Remarkably, heterocycle-containing substrates can be employed, thus expanding the scope of radical C-O cyclization reaction. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. ELECTROCHEMICAL POWER FOR TRANSPORTATION

    Energy Technology Data Exchange (ETDEWEB)

    Cairns, Elton J.; Hietbrink, Earl H.

    1981-01-01

    This section includes some historical background of the rise and fall and subsequent rebirth of the electric vehicle; and a brief discussion of current transportation needs, and environmental and energy utilization issues that resulted in the renewed interest in applying electrochemical energy conversion technology to electric vehicle applications. Although energy utilization has evolved to be the most significant and important issue, the environmental issue will be discussed first in this section only because of its chronological occurrence. The next part of the chapter is a review of passenger and commercial electric vehicle technology with emphasis on vehicle design and demonstrated performance of vehicles with candidate power sources being developed. This is followed by a discussion of electrochemical power source requirements associated with future electric vehicles that can play a role in meeting modern transportation needs. The last part of the chapter includes first a discussion of how to identify candidate electrochemical systems that might be of interest in meeting electric vehicle power source requirements. This is then followed by a review of the current technological status of these systems and a discussion of the most significant problems that must be resolved before each candidate system can be a viable power source.

  14. 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.

  15. 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.

  16. Nanocomposites for electrochemical capacitors

    CERN Document Server

    Inamuddin

    2018-01-01

    The book explores recent developments in the area of composite applications for supercapacitor electrodes based von conducting polymers, graphene, biomass, or carbonaceous quantum dots. Synthesis strategies of composite materials and electrode preparation methods are discussed in detail.

  17. Synthesis and electrochemical characterization of LiCo1/3Fe2/3PO4/C composite using nano CoFe2O4 as precursor

    International Nuclear Information System (INIS)

    Wu, Kaipeng; Hu, Guorong; Du, Ke; Peng, Zhongdong; Cao, Yanbing

    2015-01-01

    LiCo 1/3 Fe 2/3 PO 4 /C composite was synthesized by a solid state method with CoFe 2 O 4 as the precursor and glucose as the carbon source. The composite consists of homogeneous Co–Fe distributed LiCo 1/3 Fe 2/3 PO 4 with its particles covered by nano-carbon layers, which could prevent the growth of the particles as well as form a fast path for electronic transmission during charging and discharging process. It shows excellent electrochemical performance as the cathode for lithium-ion batteries, which delivers discharge capacities of 154.6, 152.9, 135.4, 122.3, 105.2 and 91.3 mAh g −1 at 0.05, 0.1, 0.5, 1, 2 and 5 C, respectively, and retains 94.6% of its initial discharge capacity after 30 cycles at 5 C. - Highlights: • Nano CoFe 2 O 4 was prepared by a co-precipitation method. • LiCo 1/3 Fe 2/3 PO 4 /C composite was synthesized using nano CoFe 2 O 4 as a precursor. • Homogeneous Co–Fe distributed LiCo 1/3 Fe 2/3 PO 4 is obtained. • LiCo 1/3 Fe 2/3 PO 4 /C composite exhibits a quite good electrochemical performance.

  18. Study on single step solid state synthesis of WC@C nanocomposite and electrochemical stability of synthesized WC@C & Pt/WC@C for alcohol oxidation (methanol/ethanol)

    Energy Technology Data Exchange (ETDEWEB)

    Singla, Gourav, E-mail: gsinghla@gmail.com; Singh, K., E-mail: kusingh@thapar.edu; Pandey, O.P., E-mail: oppandey@thapar.edu

    2016-04-25

    WC@C nano composite was prepared by a single step solid–state reaction through in situ reduction and carburization of WO{sub 3} in the presence of Mg and activated charcoal. The XRD results and thermodynamics analysis showed that the optimization of reaction temperature facilitates the reduction as well as carburization of tungsten oxide(s) at different reaction temperature. Thermogravimetric analysis of the product was done to assess the thermal stability in air. The Raman spectroscopy was used to find out the nature (amorphous/graphitic) of carbon in the obtained phase. The N{sub 2} adsorption–desorption measurement showed a narrow pore size distribution from 3 to 4 nm with BET surface area of up to 522.5 m{sup 2}/g. TEM/HRTEM images confirmed formation of the WC nano particles with spherical morphology. Electrochemical stability of pure and platinized carbide sample (Pt/WC) has been investigated using cyclic voltammetry in acidic media for alcohol (methanol and ethanol) oxidation. - Highlights: • Tungsten carbide nano powder was synthesized using charcoal as carbon source. • Formation of WC occurs through the formation of lower tungsten oxide. • CO{sub 2}/CO ratio effect the formation of WC. • Mesoporous tungsten carbide with surface areas 522.5 m{sup 2}/g obtained by using charcoal. • Pt modified WC powder showed higher electrochemical stability.

  19. Tailoring aerogel electrodes for electrochemical applications

    Science.gov (United States)

    Sakamoto, Jeffrey Steven

    2001-07-01

    The principal theme of the dissertation research was determining the relation between aerogel electrode morphology and electrochemical performance. Issues such as electrical wiring and mass transport in transition metal oxide, aerogel electrodes were addressed and designs were tailored for electrochemical applications. Single-wall carbon nanotubes were used to form the electronically conducting network in lithium intercalation electrodes that incorporated vanadium oxide aerogel as the active material. The similarities in morphology and dimensional scale for the nanotubes and V2O5 ribbons enabled excellent electrical contact to be made between the two phases without seriously affecting the aerogel nanostructure. The electrodes exhibited specific capacities in excess of 400 mAh/g at high discharge rates and retained this level of capacity on cycling. A second research goal was to improve mass transport within the aerogel electrode by minimizing tortuosity. In this research, hierarchically ordered vanadium oxide aerogel electrodes were designed and fabricated. The electrodes have two discrete and independent levels or porosity. At one level, ordered, interconnected macropores were fabricated using the templating process. At another level, interconnected mesopores were created using sol-gel synthesis and ambient drying. Electrochemical activity towards lithium was demonstrated using cyclic voltammetry and chronopotentiometry. These data are believed to be the first to demonstrate electrochemical activity for the class of materials based on the inverse opal structure. Several Group I cations and multivalent cations were reversibly, and electrochemically reacted with vanadium oxide aerogel. The molar capacities of the Group I elements (Na+ = 3.0 moles and K+ = 2.0) were high and comparable to Li+ (3.6 moles). Interestingly, the electron equivalent capacity for Mg2+ (4.0) was higher than Li+ and agrees well with the chemical titration capacity. Galvanostatic rate

  20. Remote electrochemical sensor

    Science.gov (United States)

    Wang, J.; Olsen, K.; Larson, D.

    1997-10-14

    An electrochemical sensor is described for remote detection, particularly useful for metal contaminants and organic or other compounds. The sensor circumvents technical difficulties that previously prevented in-situ remote operations. The microelectrode, connected to a long communications cable, allows convenient measurements of the element or compound at timed and frequent intervals and instrument/sample distances of ten feet to more than 100 feet. The sensor is useful for both downhole groundwater monitoring and in-situ water (e.g., shipboard seawater) analysis. 21 figs.