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Sample records for electrochemically prepared oxidation

  1. Hydrophilic graphene surface prepared by electrochemically reduced micellar graphene oxide as a platform for electrochemical sensor.

    PubMed

    Akkarachanchainon, Nontapol; Rattanawaleedirojn, Pranee; Chailapakul, Orawon; Rodthongkum, Nadnudda

    2017-04-01

    Graphene is one of the promising hydrophobic carbon-based nanomaterials used for electrode modification in electrochemical sensor. However, hydrophobicity of graphene makes it incompatible with aqueous electrolyte solution, leading to significant impediment to the electron transfer process. Here, we aim to alter graphene property to be hydrophilicity by using an electrochemically reduced micellar graphene oxide for electrode surface modification. Then, this system was applied for the simultaneous determination of toxic pesticides (e.g. carbofuran and carbendazim). Interestingly, the modified electrode offers an improved electrochemical sensitivity, verified by a drastic increase in current signal of carbofuran (4 times) and carbendazim (12 times) compared to an unmodified electrode. Under the optimal conditions, low detection limits of carbofuran and carbendazim were found to be 10µgL(-1) and 5µgL(-1), respectively. Ultimately, this system was successfully applied for the sensitive and simultaneous determination of carbofuran and carbendazim residues in various agricultural products.

  2. Preparation, characterization, and electrochemical application of mesoporous copper oxide

    SciTech Connect

    Cheng, Liang; Shao, Mingwang; Chen, Dayan; Zhang, Yuzhong

    2010-02-15

    Mesoporous CuO was successfully synthesized via thermal decomposition of CuC{sub 2}O{sub 4} precursors. These products had ring-like morphology, which was made up of nanoparticles with the average diameter of 40 nm. The electrochemical experiments showed that the mesoporous CuO decreased the overvoltage of the electrode and increased electron transference in the measurement of dopamine.

  3. Electrochemical preparation of activated graphene oxide for the simultaneous determination of hydroquinone and catechol.

    PubMed

    Velmurugan, Murugan; Karikalan, Natarajan; Chen, Shen-Ming; Cheng, Yi-Hui; Karuppiah, Chelladurai

    2017-03-31

    This paper describes the electrochemical preparation of highly electrochemically active and conductive activated graphene oxide (aGO). Afterwards, the electrochemical properties of aGO was studied towards the simultaneous determination of hydroquinone (HQ) and catechol (CC). This aGO is prepared by the electrochemical activation of GO by various potential treatments. The resultant aGOs are examined by various physical and electrochemical characterizations. The high potential activation (1.4 to -1.5) process results a highly active GO (aGO1), which manifest a good electrochemical behavior towards the determination of HQ and CC. This aGO1 modified screen printed carbon electrode (SPCE) was furnished the sensitive detection of HQ and CC with linear concentration range from 1 to 312μM and 1 to 350μM. The aGO1 modified SPCE shows the lowest detection limit of 0.27μM and 0.182μM for the HQ and CC, respectively. The aGO1 modified SPCE reveals an excellent selectivity towards the determination of HQ and CC in the presence of 100 fold of potential interferents. Moreover, the fabricated disposable aGO1/SPCE sensor was demonstrated the determination of HQ and CC in tap water and industrial waste water.

  4. The sensor based on oxidized multi-walled carbon nanotubes prepared by electrochemical method and its application

    NASA Astrophysics Data System (ADS)

    Song, Y. Z.; Yang, L.; Jiang, Q. Y.

    2015-07-01

    The sensor based on oxidized multi-walled carbon nanotubes was prepared by electrochemical method. The behavior of norepinephrine tartrate at the modified electrode was studied. It was demonstrated that modified sensor is a good electrocatalyst for norepinephrine tartrate.

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

    SciTech Connect

    Han, Kun; Miao, Peng; Tang, Yuguo; Tong, Hui; Zhu, Xiaoli; Liu, Tao; Cheng, Wenbo

    2014-02-03

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

  6. Preparation and Characterization of a PEDOT-Manganese Oxide Composite, and Its Application to Electrochemical Sensing

    NASA Astrophysics Data System (ADS)

    Arena, A.

    2016-03-01

    Stable and transparent aqueous dispersions of a hybrid organic-inorganic composite, are prepared by electrochemically doping Manganese Oxide into Polyethylendioxythiophene (PEDOT). Films deposited from the PEDOT-MnOx dispersions, are characterized by means of electrical and optical measurements, and by means of Atomic Force Microscopy (AFM) investigations. The PEDOT-MnOx composite is then used to modify one of the gold electrodes of a simple electrochemical cell, in which Nafion is used as a solid electrolyte. The cell is characterized using time domain electrical measurements. It is found that distinguishable redox peaks arise in the current-voltage loops of the cell, as nanomolar amounts of either acetic acid and ammonia, are added to the deionized water into which the cell is immersed. The intensity of such current peaks, is linearly related to the concentration of the analytes, in the nanomolar range of concentrations.

  7. Electrochemical oxidation of cholesterol

    PubMed Central

    2015-01-01

    Summary Indirect cholesterol electrochemical oxidation in the presence of various mediators leads to electrophilic addition to the double bond, oxidation at the allylic position, oxidation of the hydroxy group, or functionalization of the side chain. Recent studies have proven that direct electrochemical oxidation of cholesterol is also possible and affords different products depending on the reaction conditions. PMID:25977713

  8. Facile and novel electrochemical preparation of a graphene-transition metal oxide nanocomposite for ultrasensitive electrochemical sensing of acetaminophen and phenacetin

    NASA Astrophysics Data System (ADS)

    Jiang, Lin; Gu, Shuqing; Ding, Yaping; Jiang, Feng; Zhang, Zhen

    2013-12-01

    A facile and novel preparation strategy based on electrochemical techniques for the fabrication of electrodeposited graphene (EGR) and zinc oxide (ZnO) nanocomposite was developed. The morphology and structure of the EGR-based nanocomposite were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (XPS) and Raman spectroscopy. Meanwhile, the electrochemical performance of the nanocomposite was demonstrated with cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Due to the synergistic effect of EGR and ZnO nanoparticles, an ultrasensitive electrochemical sensor for acetaminophen (AC) and phenacetin (PCT) was successfully fabricated. The linearity ranged from 0.02 to 10 μM for AC and 0.06 to 10 μM for PCT with high sensitivities of 54 295.82 μA mM-1 cm2 for AC and 21 344.66 μA mM-1 cm2 for PCT, respectively. Moreover, the practical applicability was validated to be reliable and desirable in pharmaceutical detections. The excellent results showed the promise of the proposed preparation strategy of EGR-transition metal oxide nanocomposite in the field of electroanalytical chemistry.A facile and novel preparation strategy based on electrochemical techniques for the fabrication of electrodeposited graphene (EGR) and zinc oxide (ZnO) nanocomposite was developed. The morphology and structure of the EGR-based nanocomposite were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (XPS) and Raman spectroscopy. Meanwhile, the electrochemical performance of the nanocomposite was demonstrated with cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Due to the synergistic effect of EGR and ZnO nanoparticles, an ultrasensitive electrochemical sensor for acetaminophen (AC) and phenacetin (PCT) was successfully fabricated. The linearity ranged from 0.02 to 10 μM for AC and 0.06 to 10

  9. Sustained Release of a Monoclonal Antibody from Electrochemically Prepared Mesoporous Silicon Oxide

    PubMed Central

    Andrew, Jennifer S.; Anglin, Emily J.; Wu, Elizabeth C.; Chen, Michelle Y.; Cheng, Lingyun; Freeman, William R.; Sailor, Michael J.

    2011-01-01

    Nanostructured mesoporous silica (SiO2) films are used to load and release the monoclonal antibody bevacizumab (Avastin) in vitro. A biocompatible and biodegradable form of mesoporous SiO2 is prepared by electrochemical etching of single crystalline Si, followed by thermal oxidation in air at 800 °C. Porous SiO2 exhibits a negative surface charge at physiological pH (7.4), allowing it to spontaneously adsorb the positively charged antibody from an aqueous phosphate buffered saline solution. This electrostatic adsorption allows bevacizumab to be concentrated by >100× (300 mg bevacziumab per gram of porous SiO2 when loaded from a 1 mg mL−1 solution of bevacziumab). Drug loading is monitored by optical interferometric measurements of the thin porous film. A two-component Bruggeman effective medium model is employed to calculate percent porosity and film thickness, and is further used to determine the extent of drug loading into the porous SiO2 film. In vitro drug release profiles are characterized by an enzyme-linked immunosorbent assay (ELISA), which confirms that the antibody is released in its active, VEGF-binding form. The nanostructured delivery system described here provides a sustained release of the monoclonal antibody where approximately 98% of drug is released over a period of one month. PMID:21274422

  10. Solid state tungsten oxide hydrate/tin oxide hydrate electrochromic device prepared by electrochemical reactions

    NASA Astrophysics Data System (ADS)

    Nishiyama, Kentaro; Matsuo, Ryo; Sasano, Junji; Yokoyama, Seiji; Izaki, Masanobu

    2017-03-01

    The solid state electrochromic device composed of tungsten oxide hydrate (WO3(H2O)0.33) and tin oxide hydrate (Sn(O,OH)) has been constructed by anodic deposition of WO3(H2O)0.33 and Sn(O,OH) layers and showed the color change from clear to blue by applying voltage through an Au electrode.

  11. Fabrication of Fe2O3 nanoflakes-based electrochemical solar cells prepared by facile thermal oxidation

    NASA Astrophysics Data System (ADS)

    Rashid, Norhana Mohamed; Kishi, Naoki; Soga, Tetsuo

    2016-06-01

    A Fe2O3 nanoflakes-based solar cell was successfully prepared by thermal oxidation of iron film on FTO glass. The short circuit current density (Jsc) of the cell increased with annealing time while the open circuit voltage was saturated after 1 h. This enhancement was caused by the increased surface area of the nanoflakes and improved electron transfer through the (110) crystal plane in the Fe2O3-based electrochemical solar cell. The overall photovoltaic performance significantly increased with ruthenium dye, which likely suppressed carrier recombination on the Fe2O3 surface.

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

    NASA Astrophysics Data System (ADS)

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

    2013-12-01

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

  13. Nickel hydroxide nanoparticles-reduced graphene oxide nanosheets film: layer-by-layer electrochemical preparation, characterization and rifampicin sensory application.

    PubMed

    Rastgar, Shokoufeh; Shahrokhian, Saeed

    2014-02-01

    Electrochemical deposition, as a well-controlled synthesis procedure, has been used for subsequently layer-by-layer preparation of nickel hydroxide nanoparticle-reduced graphene oxide nanosheets (Ni(OH)2-RGO) on a graphene oxide (GO) film pre-cast on a glassy carbon electrode surface. The surface morphology and nature of the nano-hybrid film (Ni(OH)2-RGO) was thoroughly characterized by scanning electron and atomic force microscopy, spectroscopy and electrochemical techniques. The modified electrode appeared as an effective electro-catalytic model for analysis of rifampicin (RIF) by using linear sweep voltammetry (LSV). The prepared modified electrode exhibited a distinctly higher activity for electro-oxidation of RIF than either GO, RGO nanosheets or Ni(OH)2 nanoparticles. Enhancement of peak currents is ascribed to the fast heterogeneous electron transfer kinetics that arise from the synergistic coupling between the excellent properties of RGO nanosheets (such as high density of edge plane sites, subtle electronic characteristics and attractive π-π interaction) and unique properties of metal nanoparticles. Under the optimized analysis conditions, the modified electrode showed two oxidation processes for rifampicin at potentials about 0.08 V (peak I) and 0.69 V (peak II) in buffer solution of pH 7.0 with a wide linear dynamic range of 0.006-10.0 µmol L(-1) and 0.04-10 µmol L(-1) with a detection limit of 4.16 nmol L(-1) and 2.34 nmol L(-1) considering peaks I and II as an analytical signal, respectively. The results proved the efficacy of the fabricated modified electrode for simple, low cost and highly sensitive medicine sensor well suited for the accurate determinations of trace amounts of rifampicin in the pharmaceutical and clinical preparations.

  14. Electrochemical preparation of nickel and copper oxides-decorated graphene composite for simultaneous determination of dopamine, acetaminophen and tryptophan.

    PubMed

    Liu, Bingdi; Ouyang, Xiaoqian; Ding, Yaping; Luo, Liqing; Xu, Duo; Ning, Yanqun

    2016-01-01

    In the present work, transition metal oxides decorated graphene (GR) have been fabricated for simultaneous determination of dopamine (DA), acetaminophen (AC) and tryptophan (Trp) using square wave voltammetry. Electro-deposition is a facile preparation strategy for the synthesis of nickel oxide (NiO) and copper oxide (CuO) nanoparticles. GR can be modified by using citric acid to produce more functional groups, which is conducive to the deposition of dispersed metal particles. The morphologies and interface properties of the obtained NiO-CuO/GR nanocomposite were examined by scanning electron microscopy, energy dispersive X-ray spectroscopy and Raman spectroscopy. Moreover, the electrochemical performances of the composite film were investigated by cyclic voltammetry and electrochemical impedance spectroscopy. The modified electrode exhibited that the linear response ranges for detecting DA, AC and Trp were 0.5-20 μM, 4-400 μM and 0.3-40 μM, respectively, and the detection limits were 0.17 μM, 1.33 μM and 0.1 μM (S/N=3). Under optimal conditions, the sensor displayed high sensitivity, excellent stability and satisfactory results in real samples analysis.

  15. Assessment of Electrodes Prepared from Wafers of Boron-doped Diamond for the Electrochemical Oxidation of Waste Lubricants

    SciTech Connect

    Taylor, G.T.; Sullivan, I.A.; Newey, A.W.E.

    2006-07-01

    Electrochemical oxidation using boron-doped diamond electrodes is being investigated as a treatment process for radioactively contaminated oily wastes. Previously, it was shown that electrodes coated with a thin film of diamond were able to oxidise a cutting oil but not a mineral oil. These tests were inconclusive, because the electrodes lost their diamond coating during operation. Accordingly, an electrode prepared from a 'solid' wafer of boron-doped diamond is being investigated to determine whether it will oxidise mineral oils. The electrode has been tested with sucrose, a cutting oil and an emulsified mineral oil. Before and after each test, the state of the electrode was assessed by cyclic voltammetry with the ferro/ferricyanide redox couple. Analysis of the cyclic voltammogram suggested that material accumulated on the surface of the electrode during the tests. The magnitude of the effect was in the order: - emulsified mineral oil > cutting oil > sucrose. Despite this, the results indicated that the electrode was capable of oxidising the emulsified mineral oil. Confirmatory tests were undertaken in the presence of alkali to trap the carbon dioxide, but they had to be abandoned when the adhesive holding the diamond in the electrode was attacked by the alkali. Etching of the diamond wafer was also observed at the end of the tests. Surface corrosion is now regarded as an intrinsic part of the electrochemical oxidation on diamond, and it is expected that the rate of attack will determine the service life of the electrodes. (authors)

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

    NASA Astrophysics Data System (ADS)

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

    2014-10-01

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

  17. A Facile Electrochemical Preparation of Reduced Graphene Oxide@Polydopamine Composite: A Novel Electrochemical Sensing Platform for Amperometric Detection of Chlorpromazine

    NASA Astrophysics Data System (ADS)

    Palanisamy, Selvakumar; Thirumalraj, Balamurugan; Chen, Shen-Ming; Wang, Yi-Ting; Velusamy, Vijayalakshmi; Ramaraj, Sayee Kannan

    2016-09-01

    We report a novel and sensitive amperometric sensor for chlorpromazine (CPZ) based on reduced graphene oxide (RGO) and polydopamine (PDA) composite modified glassy carbon electrode. The RGO@PDA composite was prepared by electrochemical reduction of graphene oxide (GO) with PDA. The RGO@PDA composite modified electrode shows an excellent electro-oxidation behavior to CPZ when compared with other modified electrodes such as GO, RGO and GO@PDA. Amperometric i-t method was used for the determination of CPZ. Amperometry result shows that the RGO@PDA composite detects CPZ in a linear range from 0.03 to 967.6 μM. The sensor exhibits a low detection limit of 0.0018 μM with the analytical sensitivity of 3.63 ± 0.3 μAμM-1 cm-2. The RGO@PDA composite shows its high selectivity towards CPZ in the presence of potentially interfering drugs such as metronidazole, phenobarbital, chlorpheniramine maleate, pyridoxine and riboflavin. In addition, the fabricated RGO@PDA modified electrode showed an appropriate recovery towards CPZ in the pharmaceutical tablets.

  18. A Facile Electrochemical Preparation of Reduced Graphene Oxide@Polydopamine Composite: A Novel Electrochemical Sensing Platform for Amperometric Detection of Chlorpromazine.

    PubMed

    Palanisamy, Selvakumar; Thirumalraj, Balamurugan; Chen, Shen-Ming; Wang, Yi-Ting; Velusamy, Vijayalakshmi; Ramaraj, Sayee Kannan

    2016-09-21

    We report a novel and sensitive amperometric sensor for chlorpromazine (CPZ) based on reduced graphene oxide (RGO) and polydopamine (PDA) composite modified glassy carbon electrode. The RGO@PDA composite was prepared by electrochemical reduction of graphene oxide (GO) with PDA. The RGO@PDA composite modified electrode shows an excellent electro-oxidation behavior to CPZ when compared with other modified electrodes such as GO, RGO and GO@PDA. Amperometric i-t method was used for the determination of CPZ. Amperometry result shows that the RGO@PDA composite detects CPZ in a linear range from 0.03 to 967.6 μM. The sensor exhibits a low detection limit of 0.0018 μM with the analytical sensitivity of 3.63 ± 0.3 μAμM(-1 )cm(-2). The RGO@PDA composite shows its high selectivity towards CPZ in the presence of potentially interfering drugs such as metronidazole, phenobarbital, chlorpheniramine maleate, pyridoxine and riboflavin. In addition, the fabricated RGO@PDA modified electrode showed an appropriate recovery towards CPZ in the pharmaceutical tablets.

  19. A Facile Electrochemical Preparation of Reduced Graphene Oxide@Polydopamine Composite: A Novel Electrochemical Sensing Platform for Amperometric Detection of Chlorpromazine

    PubMed Central

    Palanisamy, Selvakumar; Thirumalraj, Balamurugan; Chen, Shen-Ming; Wang, Yi-Ting; Velusamy, Vijayalakshmi; Ramaraj, Sayee Kannan

    2016-01-01

    We report a novel and sensitive amperometric sensor for chlorpromazine (CPZ) based on reduced graphene oxide (RGO) and polydopamine (PDA) composite modified glassy carbon electrode. The RGO@PDA composite was prepared by electrochemical reduction of graphene oxide (GO) with PDA. The RGO@PDA composite modified electrode shows an excellent electro-oxidation behavior to CPZ when compared with other modified electrodes such as GO, RGO and GO@PDA. Amperometric i-t method was used for the determination of CPZ. Amperometry result shows that the RGO@PDA composite detects CPZ in a linear range from 0.03 to 967.6 μM. The sensor exhibits a low detection limit of 0.0018 μM with the analytical sensitivity of 3.63 ± 0.3 μAμM–1 cm–2. The RGO@PDA composite shows its high selectivity towards CPZ in the presence of potentially interfering drugs such as metronidazole, phenobarbital, chlorpheniramine maleate, pyridoxine and riboflavin. In addition, the fabricated RGO@PDA modified electrode showed an appropriate recovery towards CPZ in the pharmaceutical tablets. PMID:27650697

  20. In situ one-pot preparation of reduced graphene oxide/polyaniline composite for high-performance electrochemical capacitors

    NASA Astrophysics Data System (ADS)

    Chen, Nali; Ren, Yapeng; Kong, Peipei; Tan, Lin; Feng, Huixia; Luo, Yongchun

    2017-01-01

    Reduced graphene oxide/polyaniline (rGO/PANI) composites are prepared through an effective in situ one-pot synthesis route that includes the reduction of graphene oxide (GO) by aniline under weak alkali condition via hydrothermal method and then followed by in situ polymerization of aniline. X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, ultraviolet-visible spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscope and transmission electron microscope are employed to reveal that GO is successfully reduced by aniline under weak alkali condition and PANI can be deposited on the surfaces of reduced graphene oxide (rGO) sheets. The effect of rGO is optimized by tuning the mass ratios of aniline to GO to improve the electrochemical performance of rGO/PANI composites. The maximum specific capacitance of rGO/PANI composites achieves 524.4 F/g with a mass ratio of aniline to GO 10:1 at a current density of 0.5 A/g, in comparison to the specific capacitance of 397 F/g at the same current density of pure PANI. Particularly, the specific capacity retention rate is 81.1% after 2000 cycles at 100 mv/s scan rate, which is an improvement over that of pure PANI (55.5%).

  1. Preparation of graphene/vanadium oxide nanocomposite monolith and its electrochemical performance

    SciTech Connect

    Deng, Lingjuan; Ma, Zhanying; Li, Xiaobo; Fan, Guang

    2015-10-15

    Graphical Abstract: Graphene/V{sub 2}O{sub 5}(G/V{sub 2}O{sub 5}) nanocomposite monolith is prepared in a mixture of ammonium vanadate, acetic acid and graphite oxide by one-step hydrothermal technology. Owing to the novel structure of ultralong V{sub 2}O{sub 5} nanobelts interpenetrated between the G nanosheets, the G/V{sub 2}O{sub 5} nanocomposite electrode shows higher specific capacitances and better cycle stability than those of G and V{sub 2}O{sub 5} electrodes for supercapaciors and lithium ion battaries. - Highlights: • G/V{sub 2}O{sub 5} nanocomposite monolith is prepared by one-step hydrothermal technology. • G/V{sub 2}O{sub 5} nanocomposite electrode shows much excellent capacitive property. • G/V{sub 2}O{sub 5} nanocomposite exhibits more stable cycle performance. - Abstract: Graphene/vanadium oxide nanocomposite (G/V{sub 2}O{sub 5}) monolith is prepared via a simple hydrothermal process. Owing to the intimate contact between the V{sub 2}O{sub 5} nanobelts and graphene nanosheets in the monolith, the nanocomposite shows excellent electric conductivity, and therefore makes the electrode–electrolyte contact better and Li{sup +} diffusion faster. A high specific capacitance of 163 F g{sup −1} has been achieved for G/V{sub 2}O{sub 5} electrode in 0.5 mol L{sup −1} K{sub 2}SO{sub 4} solution. The G/V{sub 2}O{sub 5} nanocomposite exhibits excellent cyclic performance with nearly 80% capacity retention at a current density of 5 A g{sup −1} in a testing range of 1000 cycles. Moreover, G/V{sub 2}O{sub 5} nanocomposite exhibits excellent discharge properties and cycle stability as an anode material for lithium ion batteries. The initial capacity is 1100 mAh g{sup −1} and the reversible capacity of 530 mAh g{sup −1} is maintained after 100 cycles at a current density of 50 mA g{sup −1}.

  2. Electrochemical oxidation of methylenedioxyamphetamines.

    PubMed

    Squella, J A; Cassels, B K; Arata, M; Bavestrello, M P; Nuñez-Vergara, L J

    1993-09-01

    Four amphetamine derivatives bearing a methylenedioxy group at positions 3 and 4 of the benzene ring and differing in their substitution at C(6) were studied by differential pulse voltammetry in aqueous media. These experiments showed a single oxidation peak for the C(6)-H, -Br and -Cl compounds, while the C(6)-NO(2) analogue was not oxidized. The oxidation peak is interpreted as due to the removal of one electron from the aromatic electrophore with formation of a radical cation stabilized by the dioxole ring. The linear relationship between the peak current and the concentration of the derivatives is appropriate for development of a quantitative method for their determination. pK' values were determined using both electrochemical and spectrophotometric methods.

  3. Influence of concentration and volume of precursor on the electrochemical properties of vanadium oxide thin films prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Ingole, R. S.; Fugare, B. Y.; Lokhande, B. J.

    2016-04-01

    Vanadium oxide (V2O5) thin films have been prepared by spray pyrolysis using different concentrations and volumes of precursor solution via aqueous route at 673K deposition temperature. The influences of concentration and volume on the structural, morphological and electrochemical properties of the deposited samples are studied well. X - ray diffraction study shows orthorhombic crystal structure with V2O5 phase, confirmed by FTIR spectroscopy. Scanning electron microscopy shows granular, homogeneous and dense surface morphology. Cyclic voltammetery of all samples carried at all scan rates. Samples prepared using 0.05M, 40 ml of precursor solution shows highest specific capacitance 428.25 F/gm at 5 mV/s, Charge discharge behavior exhibits specific energy 18.73 Wh/kg, specific power 36.00 kW/kg, columbic efficiency 87.50 %. Impedance spectroscopy study was carried in the frequency range 1mHz - 1MHz, reveals pseudocapacitive behavior of the electrode exhibiting internal resistance 1.34 ohm.

  4. Influence of concentration and volume of precursor on the electrochemical properties of vanadium oxide thin films prepared by spray pyrolysis

    SciTech Connect

    Ingole, R. S.; Fugare, B. Y.; Lokhande, B. J.

    2016-04-13

    Vanadium oxide (V{sub 2}O{sub 5}) thin films have been prepared by spray pyrolysis using different concentrations and volumes of precursor solution via aqueous route at 673K deposition temperature. The influences of concentration and volume on the structural, morphological and electrochemical properties of the deposited samples are studied well. X - ray diffraction study shows orthorhombic crystal structure with V{sub 2}O{sub 5} phase, confirmed by FTIR spectroscopy. Scanning electron microscopy shows granular, homogeneous and dense surface morphology. Cyclic voltammetery of all samples carried at all scan rates. Samples prepared using 0.05M, 40 ml of precursor solution shows highest specific capacitance 428.25 F/gm at 5 mV/s, Charge discharge behavior exhibits specific energy 18.73 Wh/kg, specific power 36.00 kW/kg, columbic efficiency 87.50 %. Impedance spectroscopy study was carried in the frequency range 1mHz – 1MHz, reveals pseudocapacitive behavior of the electrode exhibiting internal resistance 1.34 ohm.

  5. Hydrothermal preparation of reduced graphene oxide-silver nanocomposite using Plectranthus amboinicus leaf extract and its electrochemical performance.

    PubMed

    Zheng, Yuhong; Wang, Aiwu; Cai, Wen; Wang, Zhong; Peng, Feng; Liu, Zhong; Fu, Li

    2016-12-01

    Graphene based nanocomposites are receiving increasing attention in many fields such as material chemistry, environmental science and pharmaceutical science. In this study, a facial synthesis of a reduced graphene oxide-silver nanocomposite (RGO-Ag) was carried out from Plectranthus amboinicus leaf extract. The synthesized nanocomposite was characterized by using X-ray diffraction, scanning electron microscope, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscope and UV-vis spectroscopy for structural confirmation. The reduction of graphene oxide and silver ions was achieved simultaneously due to the reducibility of the Plectranthus amboinicus leaf extract. We further investigated the electrochemical properties of the biosynthesized RGO-Ag nanocomposite. A nonenzymatic H2O2 electrochemical sensor was shown to be successfully fabricated by using biosynthesized RGO-Ag nanocomposite. Moreover, the fabricated electrochemical sensor also showed good selectivity.

  6. Preparation of AAO-CeO2 nanotubes and their application in electrochemical oxidation desulfurization of diesel.

    PubMed

    Du, Xiaoqing; Yang, Yumeng; Yi, Chenxi; Chen, Yu; Cai, Chao; Zhang, Zhao

    2017-02-10

    The coaxial arrays of AAO-CeO2 NTs have been successfully galvanostatically deposited on an anode, characterized and adopted as a catalyst for removing organic sulfurs from diesel. The influence of the main electrochemical oxidation factors on the efficiency of desulfurization have also been investigated. The results show that the fabrication process of AAO-CeO2 NTs is accompanied by the formation of a new phase, namely Al3Ce, and the main oxidation products of the diesel are soluble inorganic sulphides, especially Ce2(SO4)3. When compared with dibenzothiophene and 4, 6-dimethyldibenzothiophene, benzothiophene is much more easily removed, with a removal efficiency that reaches 87.2%. Finally, a possible electrochemical oxidation desulfurization pathway for diesel is proposed.

  7. Preparation of AAO-CeO2 nanotubes and their application in electrochemical oxidation desulfurization of diesel

    NASA Astrophysics Data System (ADS)

    Du, Xiaoqing; Yang, Yumeng; Yi, Chenxi; Chen, Yu; Cai, Chao; Zhang, Zhao

    2017-02-01

    The coaxial arrays of AAO-CeO2 NTs have been successfully galvanostatically deposited on an anode, characterized and adopted as a catalyst for removing organic sulfurs from diesel. The influence of the main electrochemical oxidation factors on the efficiency of desulfurization have also been investigated. The results show that the fabrication process of AAO-CeO2 NTs is accompanied by the formation of a new phase, namely Al3Ce, and the main oxidation products of the diesel are soluble inorganic sulphides, especially Ce2(SO4)3. When compared with dibenzothiophene and 4, 6-dimethyldibenzothiophene, benzothiophene is much more easily removed, with a removal efficiency that reaches 87.2%. Finally, a possible electrochemical oxidation desulfurization pathway for diesel is proposed.

  8. Preparation and characterization of zinc oxide nanoparticles and their sensor applications for electrochemical monitoring of nucleic acid hybridization.

    PubMed

    Yumak, Tugrul; Kuralay, Filiz; Muti, Mihrican; Sinag, Ali; Erdem, Arzum; Abaci, Serdar

    2011-09-01

    In this study, ZnO nanoparticles (ZNP) of approximately 30 nm in size were synthesized by the hydrothermal method and characterized by X-ray diffraction (XRD), Braun-Emmet-Teller (BET) N2 adsorption analysis and transmission electron microscopy (TEM). ZnO nanoparticles enriched with poly(vinylferrocenium) (PVF+) modified single-use graphite electrodes were then developed for the electrochemical monitoring of nucleic acid hybridization related to the Hepatitis B Virus (HBV). Firstly, the surfaces of polymer modified and polymer-ZnO nanoparticle modified single-use pencil graphite electrodes (PGEs) were characterized using scanning electron microscopy (SEM). The electrochemical behavior of these electrodes was also investigated using differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy (EIS). Subsequently, the polymer-ZnO nanoparticle modified PGEs were evaluated for the electrochemical detection of DNA based on the changes at the guanine oxidation signals. Various modifications in DNA oligonucleotides and probe concentrations were examined in order to optimize the electrochemical signals that were generated by means of nucleic acid hybridization. After the optimization studies, the sequence-selective DNA hybridization was investigated in the case of a complementary amino linked probe (target), or noncomplementary (NC) sequences, or target and mismatch (MM) mixture in the ratio of (1:1).

  9. Preparation of cribriform sheet-like carbon-coated zinc oxide with improved electrochemical performance

    NASA Astrophysics Data System (ADS)

    Huang, Jianhang; Yang, Zhanhong; Xie, Xiaoe; Feng, Zhaobin; Zhang, Zheng

    2015-09-01

    Cribriform sheet-like carbon-coated ZnO are prepared using pyrrole as the carbon source. It is found that a sheet-like precursor will form when polymerizing pyrrole in the presence of ZnO particles. After the carbonization of precursor, cribriform sheet-like carbon-coated ZnO can be obtained. Morphology and structure analysis of as-prepared carbon-coated ZnO is conducted by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The carbon overlayer not only present a barrier layer on the surface of the ZnO particles, which keeps relative high discharge capacity by inhibiting the active materials in electrode from dissolving into electrolyte, but also modify the surface status of ZnO particles so as to obtain more uniform current distribution and improved conductivity. As a result, when evaluated as an anode material for Zn/Ni cell, carbon-coated ZnO exhibit a more stable cycle performance than bare ZnO electrode.

  10. Electrochemical Preparation of Polymer Electrodes.

    DTIC Science & Technology

    1986-10-18

    A %... %’ a C- ’C ’.- ’ ", -" . ’.:. "’’’ .- ",. ". - - - . . Mir __ .-~ . _. A - - - . -r. x.-. -", _ . - - -e , . 0: Unclassified SECURITY ...CLASSIFICATION OF THIS. PAGE % ’OC’ AD-A 173 984 Ia. REPORT SECURITY CLASSIFICATION 2a, SECURITY CLASSIFICATION AUT R1 3. DISTRIBUTION/AVAILABILITY OF REPORT...PROGRAM PROJECT TASK WORK UNIT ELEMENT NO. NO. NO ACCESSION NO 11. TITLE (Include Security Classification) Electrochemical Preparation of Polymer

  11. Direct electrochemical oxidation of polyacrylates.

    PubMed

    Bellagamba, Riccardo; Comninellis, Christos; Vatistas, Nicolaos

    2002-10-01

    A promising elimination treatment of non-biodegradable organic pollutants is the direct electro-oxidation. In this work has been proposed the electrochemical elimination of polyacrylates by using boron-doped diamond (BDD) as anodic material. The complete elimination of organic contaminants has been obtained and this is the first case of successful electrochemical treatment of polymeric and bio-refractory species. The tests of the electrochemical oxidation have been conducted at constant current conditions and a complete elimination of organic species has been reached. The decrease of the COD value with time follows the behaviour of an ideal anode as in the case of low molecular organic compounds.

  12. Electrochemically synthesized ordered TiO2 and platinum nanocomposite electrode: preparation, characterization, and application to photoelectrocatalytic methanol oxidation

    SciTech Connect

    Li, Zhizhou; Cui, Xiaoli; Lin, Yuehe

    2009-04-01

    In this work, the nanocomposite electrodes consisting of Pt and TiO2 nanotubular arrays have been synthesized, and the morphologies, structural, and photo-electrochemical properties of the electrodes are characterized by SEM, XRD, and electrochemical methods. Highly ordered TiO2 nanotubular arrays can be obtained through anodization of titanium. The platinum nanoparticles are electrodeposited into TiO2 nanotubes by a chronopotentiometry method. Cyclic voltammetry and XRD measurements can confirm the presence of platinum in this nanocomposite electrode. The nanostructural electrode greatly improved performances for methanol oxidation under UV-Vis illumination compared to that without illumination. An enhancement of 58% in the current density has been observed upon illumination with UV-Vis light irradiance at an intensity of 50 mW/cm2. The improved performance of the TiO2/Pt nanocomposite electrode results from a enhanced methanol oxidation by photo-generated holes in the TiO2 nanoarrays under illumination and a synergistic effectiveness between TiO2 and Pt nanoparticles.

  13. Electrochemically reduced graphene oxide / sulfonated polyether ether ketone composite membrane for electrochemical applications

    NASA Astrophysics Data System (ADS)

    Seetharaman, S.; Ramya, K.; Dhathathreyan, K. S.

    2013-06-01

    A simple and effective method for the preparation of sulfonated polyether ether ketone (SPEEK) based composites with electrochemical reduced graphene oxide (EGO) as inorganic fillers has been described. The resulting dispersions are homogeneous and the cast membranes show significant improvement on tensile strength and thermal properties. It has high ionic conductivity and is cost effective making it a promising alternative membrane for electrochemical applications.

  14. Electrochemical post-treatment of infinite coordination polymers: an effective route to preparation of Pd nanoparticles supported onto carbon nanotubes with enhanced electrocatalytic activity toward ethanol oxidation.

    PubMed

    Ren, Lin; Yang, Lifen; Yu, Ping; Wang, Yuexiang; Mao, Lanqun

    2013-11-13

    This study describes an effective method to prepare highly dispersed palladium nanoparticles supported onto single-walled carbon nanotubes (SWNTs) with high electrocatalytic activity toward the oxidation of ethanol. This method is essentially based on electrochemical post-treatment of Pd-based infinite coordination polymer (ICP). The Pd-based ICP is synthesized through the coordination reaction between Zn(2+) and metallo-Schiff base (MSB) to form Zn-MSB-Zn (ZMZ) ICP that precipitates from ethyl ether. The as-formed Zn-MSB-Zn ICP is then subjected to an ion-exchange reaction with Pd(2+) to obtain the Zn-MSB-Pd (ZMP) ICP. To prepare Pd/SWNT nanocomposite, the ZMP ICP is mixed into the SWNT dispersion in N-dimethylformamide (DMF) to form a homogeneous dispersion that is then drop-coated onto a glassy carbon (GC) electrode. Electrochemical post-treatment of ZMP ICP to form Pd/SWNT nanocomposite is thus performed by polarizing the coated electrode at -0.2 V for 600 s in 0.5 M H2SO4. The results obtained with scanning electron microscopy (SEM) and transmission electron microscopy (TEM) reveal that the resulting Pd nanoparticles are highly dispersed onto SWNTs and the particles size are small and narrowly distributed (2.12 ± 0.32 nm). X-ray photoelectron spectroscopy (XPS) analysis shows that, after the electrochemical post-treatment, no detectable ZMP ICP precursors are left on the surface of SWNTs. The electrocatalytic activity of the as-formed Pd/SWNT nanocomposite toward ethanol oxidation is investigated by cyclic voltammetry and chronoamperometry. The results show that the Pd/SWNT nanocomposite prepared here shows a more negative potential and higher mass catalytic activity, as well as higher stability for the oxidation of ethanol than the commercial Pd/C catalyst. This work demonstrates a novel approach to the formation of ultrasmall and highly dispersed Pd/SWNT nanocomposite with enhanced electrocatalytic activity toward ethanol oxidation.

  15. Electrochemical oxidation of chemical weapons

    SciTech Connect

    Surma, J.E.

    1994-05-01

    Catalyzed electrochemical oxidation (CEO), a low-temperature electrochemical oxidation technique, is being examined for its potential use in destroying chemical warfare agents. The CEO process oxidizes organic compounds to form carbon dioxide and water. A bench-scale CEO system was used in three separate tests sponsored by the US Department of Energy`s (DOE) Office of Intelligence and National Security through the Advanced Concepts Program. The tests examined the effectiveness of CEO in destroying sarin (GB), a chemical nerve agent. The tests used 0.5 mL, 0.95 mL, and 1.0 mL of GB, corresponding to 544 mg, 816 mg, and 1,090 mg, respectively, of GB. Analysis of the off gas showed that, under continuous processing of the GB agent, destruction efficiencies of better than six 9s (99.9999% destroyed) could be achieved.

  16. Solid oxide electrochemical reactor science.

    SciTech Connect

    Sullivan, Neal P.; Stechel, Ellen Beth; Moyer, Connor J.; Ambrosini, Andrea; Key, Robert J.

    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.

  17. Electrochemical oxidation for landfill leachate treatment

    SciTech Connect

    Deng, Yang Englehardt, James D.

    2007-07-01

    This paper aims at providing an overview of electrochemical oxidation processes used for treatment of landfill leachate. The typical characteristics of landfill leachate are briefly reviewed, and the reactor designs used for electro-oxidation of leachate are summarized. Electrochemical oxidation can significantly reduce concentrations of organic contaminants, ammonia, and color in leachate. Pretreatment methods, anode materials, pH, current density, chloride concentration, and other additional electrolytes can considerably influence performance. Although high energy consumption and potential chlorinated organics formation may limit its application, electrochemical oxidation is a promising and powerful technology for treatment of landfill leachate.

  18. Preparation and electrochemical characterization of ionic-conducting lithium lanthanum titanate oxide/polyacrylonitrile submicron composite fiber-based lithium-ion battery separators

    NASA Astrophysics Data System (ADS)

    Liang, Yinzheng; Ji, Liwen; Guo, Bingkun; Lin, Zhan; Yao, Yingfang; Li, Ying; Alcoutlabi, Mataz; Qiu, Yiping; Zhang, Xiangwu

    Lithium lanthanum titanate oxide (LLTO)/polyacrylonitrile (PAN) submicron composite fiber-based membranes were prepared by electrospinning dispersions of LLTO ceramic particles in PAN solutions. These ionic-conducting LLTO/PAN composite fiber-based membranes can be directly used as lithium-ion battery separators due to their unique porous structure. Ionic conductivities were evaluated after soaking the electrospun LLTO/PAN composite fiber-based membranes in a liquid electrolyte, 1 M lithium hexafluorophosphate (LiPF 6) in ethylene carbonate (EC)/ethyl methyl carbonate (EMC) (1:1 vol). It was found that, among membranes with various LLTO contents, 15 wt.% LLTO/PAN composite fiber-based membranes provided the highest ionic conductivity, 1.95 × 10 -3 S cm -1. Compared with pure PAN fiber membranes, LLTO/PAN composite fiber-based membranes had greater liquid electrolyte uptake, higher electrochemical stability window, and lower interfacial resistance with lithium. In addition, lithium//1 M LiPF 6/EC/EMC//lithium iron phosphate cells containing LLTO/PAN composite fiber-based membranes as the separator exhibited high discharge specific capacity of 162 mAh g -1 and good cycling performance at 0.2 C rate at room temperature.

  19. Electrochemical preparation of poly(3-methylthiophene-carbazole)/graphene oxide composite coating for the highly effective solid-phase microextraction of some fragrance.

    PubMed

    Zhang, Jie; Yang, Liu; Wu, Mian; Guo, Xiafei; Zeng, Baizhao; Zhao, Faqiong

    2017-08-15

    A poly(3-methylthiophene-carbazole)/graphene oxide composite coating was prepared on a stainless steel wire through electrochemical method. It showed high extraction efficiency, thermal stability and durability than those of corresponding single-component coatings due to the synergistic effect of different components. The resulting fiber was used for the headspace solid phase microextraction of octanal, nonanal, decanal, undecanol and dodecanol, followed by gas chromatography detection. The results showed that their GC peak areas were linear to their concentrations in the ranges of about 0.05-100μgL(-1), the detection limits were 22.6-40.5ngL(-1) (S/N=3). The run-to-run RSD was smaller than 4.5% (n=4), and the fiber-to-fiber RSD was 4.0-9.3% (n=4). The method was successfully applied to the determination of the five analytes in candy, orange fruit and flower. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Nucleophilic aromatic substitution for heteroatoms: an oxidative electrochemical approach.

    PubMed

    Gallardo, Iluminada; Guirado, Gonzalo; Marquet, Jordi

    2002-04-19

    The nucleophilic aromatic substitution for heteroatom through electrochemical oxidation of the intermediate sigma-complexes (Meisenheimer complexes) in simple nitroaromatic compounds is reported for the first time (NASX process). The studies have been carried out with hydride, cyanide, fluoride, methoxy, and ethanethiolate anions and n-butylamine as a nucleophile, at the cyclic voltammetry (CV) and preparative electrolysis level. The cyclic voltammetry experiments allow for detection and characterization of the sigma-complexes and they have led us to a proposal for the mechanism of the oxidation step. Furthermore, the power of the CV technique in the analysis of the reaction mixture throughout the whole chemical and electrochemical process is described.

  1. Effect of citric acid dosage and sintered temperature on the composition, morphology and electrochemical properties of lithium vanadium oxide prepared by a sol–gel method

    NASA Astrophysics Data System (ADS)

    Zhong, C. R.; Su, X. J.; Hou, G. L.; Liu, Z. H.; Yu, F. S.; Bi, S.; Li, H.

    2017-03-01

    A lithium vanadium oxide cathode material was synthesized via sol-gel processing using citric acid as the chelating agent. Different dosage of citric acid and sintered temperature were introduced to investigate their effects on the products composition, morphology and electrochemical properties. The results showed that the V2O3 yield was inhibited and the crystallization of grain was accelerated with the increasing dosage of citric acid. Furthermore, V2O3 was oxidized to LiV3O8 and Li0.3V2O5 with the increase of sintered temperature.

  2. Dechlorination by combined electrochemical reduction and oxidation*

    PubMed Central

    Cong, Yan-qing; Wu, Zu-cheng; Tan, Tian-en

    2005-01-01

    Chlorophenols are typical priority pollutants listed by USEPA (U.S. Environmental Protection Agency). The removal of chlorophenol could be carried out by a combination of electrochemical reduction and oxidation method. Results showed that it was feasible to degrade contaminants containing chlorine atoms by electrochemical reduction to form phenol, which was further degraded on the anode by electrochemical oxidation. Chlorophenol removal rate was more than 90% by the combined electrochemical reduction and oxidation at current of 6 mA and pH 6. The hydrogen atom is a powerful reducing agent that reductively dechlorinates chlorophenols. The instantaneous current efficiency was calculated and the results indicated that cathodic reduction was the main contributor to the degradation of chlorophenol. PMID:15909345

  3. Dechlorination by combined electrochemical reduction and oxidation.

    PubMed

    Cong, Yan-qing; Wu, Zu-cheng; Tan, Tian-en

    2005-06-01

    Chlorophenols are typical priority pollutants listed by USEPA (U.S. Environmental Protection Agency). The removal of chlorophenol could be carried out by a combination of electrochemical reduction and oxidation method. Results showed that it was feasible to degrade contaminants containing chlorine atoms by electrochemical reduction to form phenol, which was further degraded on the anode by electrochemical oxidation. Chlorophenol removal rate was more than 90% by the combined electrochemical reduction and oxidation at current of 6 mA and pH 6. The hydrogen atom is a powerful reducing agent that reductively dechlorinates chlorophenols. The instantaneous current efficiency was calculated and the results indicated that cathodic reduction was the main contributor to the degradation of chlorophenol.

  4. A facile approach to prepare crumpled CoTMPyP/electrochemically reduced graphene oxide nanohybrid as an efficient electrocatalyst for hydrogen evolution reaction

    NASA Astrophysics Data System (ADS)

    Ma, Juanjuan; Liu, Lin; Chen, Qian; Yang, Min; Wang, Danping; Tong, Zhiwei; Chen, Zhong

    2017-03-01

    Elaborate design and synthesis of efficient and stable non-Pt electrocatalysts for some renewable energy related conversion/storage processes are one of the major goals of sustainable chemistry. Herein, we report a facile method to fabricate Co porphyrin functionalized electrochemically reduced graphene oxide (CoTMPyP/ERGO) thin film by direct assembly of oppositely charged tetrakis(N-methylpyridyl) porphyrinato cobalt (CoTMPyP) and GO nanosheets under mild conditions followed by an electrochemical reduction procedure. STEM analysis confirms that CoTMPyP nanoaggregates are homogeneously distributed over the graphene surface. The electrochemical properties of CoTMPyP/ERGO were investigated by cyclic voltammetry, linear sweep voltammetry and electrochemical impedance spectroscopy. The results demonstrate that CoTMPyP/ERGO nanohybrid film can serve as excellent electrocatalyst for hydrogen evolution in alkaline solution with high activity and stability. The intimate contact and efficient electron transfer between CoTMPyP and ERGO, as well as the crumpled structure, contribute to the improvement of the electrocatalytic performance.

  5. An electrochemically reduced graphene oxide-based electrochemical immunosensing platform for ultrasensitive antigen detection.

    PubMed

    Haque, Al-Monsur Jiaul; Park, Hyejin; Sung, Daekyung; Jon, Sangyong; Choi, Sung-Yool; Kim, Kyuwon

    2012-02-21

    We present an electrochemically reduced graphene oxide (ERGO)-based electrochemical immunosensing platform for the ultrasensitive detection of an antigen by the sandwich enzyme-linked immunosorbent assay (ELISA) protocol. Graphene oxide (GO) sheets were initially deposited on the amine-terminated benzenediazonium-modified indiun tin oxide (ITO) surfaces through both electrostatic and π-π interactions between the modified surfaces and GO. This deposition was followed by the electrochemical reduction of graphene oxide (GO) for preparing ERGO-modified ITO surfaces. These surfaces were then coated with an N-acryloxysuccinimide-activated amphiphilic polymer, poly(BMA-r-PEGMA-r-NAS), through π-π stacking interactions between the benzene ring tethered to the polymer and ERGO. After covalent immobilization of a primary antibody on the polymer-modified surfaces, sandwich ELISA was carried out for the detection of an antigen by use of a horseradish peroxidase (HRP)-labeled secondary antibody. Under the optimized experimental conditions, the developed electrochemical immunosensor exhibited a linear response over a wide range of antigen concentrations with a very low limit of detection (ca. 100 fg/mL, which corresponds to ca. 700 aM). The high sensitivity of the electrochemical immunosensor may be attributed not only to the enhanced electrocatalytic activity owing to ERGO but also to the minimized background current owing to the reduced nonspecific binding of proteins.

  6. Effect of poly(ethylene oxide) on ionic conductivity and electrochemical properties of poly(vinylidenefluoride) based polymer gel electrolytes prepared by electrospinning for lithium ion batteries

    NASA Astrophysics Data System (ADS)

    Prasanth, Raghavan; Shubha, Nageswaran; Hng, Huey Hoon; Srinivasan, Madhavi

    2014-01-01

    Effect of poly(ethylene oxide) on the electrochemical properties of polymer electrolyte based on electrospun, non-woven membrane of PVdF is demonstrated. Electrospinning process parameters are controlled to get a fibrous membrane consisting of bead-free, uniformly dispersed thin fibers with diameter in the range of 1.5-1.9 μm. The membrane with good mechanical strength and porosity exhibits high uptake when activated with the liquid electrolyte of lithium salt in a mixture of organic solvents. The polymer gel electrolyte shows ionic conductivity of 4.9 × 10-3 S cm-1 at room temperature. Electrochemical performance of the polymer gel electrolyte is evaluated in Li/polymer electrolyte/LiFePO4 coin cell. Good performance with low capacity fading on charge-discharge cycling is demonstrated.

  7. Preparation of electrochemically active silicon nanotubes in highly ordered arrays.

    PubMed

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

    2013-01-01

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

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

    SciTech Connect

    Erçarıkcı, Elif; Dağcı, Kader; Topçu, Ezgi; Alanyalıoğlu, Murat

    2014-07-01

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

  9. Electrochemical Oxidation of Alkylnitro Compounds PP-1345

    DTIC Science & Technology

    2004-08-17

    dinitropropanol (DNPOH, the precursor to the energetic plasticizer BDNPA/F) yield as byproducts large amounts of chemical process waste in the form...these chemistries and the significantly large resulting waste streams requiring treatment and disposal after the manufacturing chemistry is completed...fielded materials and many others, and thus avoid their byproducts and large waste streams. This proven electrochemical oxidation technology, employed

  10. Preparation and electrochemical properties of polyaniline nanofibers using ultrasonication

    SciTech Connect

    Manuel, James; Kim, Miso; Fapyane, Deby; Chang, In Seop; Ahn, Hyo-Jun; Ahn, Jou-Hyeon

    2014-10-15

    Highlights: • Nanofibrous structured polyaniline (PANI) was prepared by simple ultrasonication. • PANI nanofibers prepared at 5 °C are uniform with an average diameter of 50 nm. • The conductivity is increased by 2 × 10{sup 8} times after doping with LiClO{sub 4}. • The cell with PANI-LiClO{sub 4} shows good cycle performance at high current densities. - Abstract: Polyaniline nanofibers have been successfully prepared by applying ultrasonic irradiation during oxidative polymerization of aniline in dilute hydrochloric acid and evaluated for suitability in lithium cells after doping with lithium perchlorate salt. Polyaniline nanofibers are confirmed by Fourier transform infrared spectroscopy, Fourier transform Raman spectroscopy, and transmission electron microscopy, and the efficiency of doping is confirmed by DC conductivity measurements at different temperatures. Electrochemical properties of nanofibers are evaluated, of which a remarkable increase in cycle stability is achieved when compared to polyaniline prepared by simple oxidative polymerization of aniline. The cell with nanofibrous polyaniline doped with LiClO{sub 4} delivers an initial discharge capacity value of 86 mA h g{sup −1} at 1 C-rate which is about 60% of theoretical capacity, and the capacity is slightly lowered during cycle and reaches 50% of theoretical capacity after 40 cycles. The cell delivers a stable and higher discharge capacity even at 2 C-rate compared to that of the cell prepared with bulk polyaniline doped with LiClO{sub 4}.

  11. Electrochemical oxygen intercalation in La 2CuO 4 prepared by nitrates method: Microstructural effects

    NASA Astrophysics Data System (ADS)

    Michel, C. R.; Casan˜-Pastor, N.

    2000-11-01

    In order to determine microstructural effects in the electrochemical oxygen intercalation for La 2CuO 4, and the relative abundance of the two superconducting phases (T c = 33 and 44K), this oxide was prepared using the nitrates method, which involves the dissolution of La and Cu oxides in nitric acid. The product was pressed as pellets. A narrow grain size distribution and a density higher than 95% ϱ T was obtained. After electrochemical oxygen intercalation, at room temperature, this material gave a main superconducting phase with T c = 33K, whereas porous pellets obtaiined from the same oxide, with intermediate grinding, gave a T c = 44K.

  12. Preparation of reliable probes for electrochemical tunneling spectroscopy.

    PubMed

    Güell, Aleix G; Díez-Pérez, Ismael; Gorostiza, Pau; Sanz, Fausto

    2004-09-01

    We present a new procedure to prepare Pt/Ir probes for electrochemical scanning tunneling microscopy (STM) and spectroscopy applications. We detail the experimental setup and the improvements over previous methods. The probes have been used successfully for measurements of tunneling spectroscopy under electrochemical control, which requires scanning the potential of the tip at high velocity. Copyright 2004 American Chemical Society

  13. Solid oxide electrochemical cell fabrication process

    DOEpatents

    Dollard, Walter J.; Folser, George R.; Pal, Uday B.; Singhal, Subhash C.

    1992-01-01

    A method to form an electrochemical cell (12) is characterized by the steps of thermal spraying stabilized zirconia over a doped lanthanum manganite air electrode tube (14) to provide an electrolyte layer (15), coating conductive particles over the electrolyte, pressurizing the outside of the electrolyte layer, feeding halide vapors of yttrium and zirconium to the outside of the electrolyte layer and feeding a source of oxygen to the inside of the electrolyte layer, heating to cause oxygen reaction with the halide vapors to close electrolyte pores if there are any and to form a metal oxide coating on and between the particles and provide a fuel electrode (16).

  14. Electrochemical and photocatalytic oxidation of hydrocarbons

    NASA Astrophysics Data System (ADS)

    Rismanchian, Azadeh

    This study demonstrates the development of a stable anode for electrochemical oxidation of hydrocarbons in solid oxide fuel cell (SOFC) and a highly active TiO2 based catalyst for photocatalytic reactions. The Ni/YSZ anode of SOFC was modified by Cu electroless plating. The catalytic activity toward H2 and CH4 oxidation were compared by the Faraday resistance (RF) obtained from the impedance spectroscopy. The RF ratio of Cu-Ni/YSZ in CH4 to H2 was greater than that of Ni/YSZ, indicating low catalytic activity of Cu-Ni/YSZ toward CH4 oxidation. The addition of Cu decreased the catalytic activity, but increased stability to 138 h in dry CH4. Characterization of the carbon type with Raman spectroscopy and temperature programmed oxidation showed that Cu formed disordered carbon rather than graphitic carbon which is the precursor to coking. Addition of CO2 to CH4 was studied as another approach to prevent coking. Electrochemical performance and mass spectrometry of the reactor effluent showed that the CH4-CO2 SOFC generated electricity from CO and H2, products of dry reforming reaction, with CO as the major contributor to current generation. CH4-CO 2 decreased the activation polarization but showed a limiting current due to the fuel depletion at the interlayer-electrolyte interface. Anode interlayer was modified by reducing the particle size to 2 mum. The fine microstructure increased the three phase boundary length and reduced the activation polarization. The pore loss in the fine microstructure resulted in diffusion limitation and a limiting current in CH4 which was eliminated by adding 4 wt% of pore former at interlayer. Further addition of pore former lowered the performance by creating discontinuity at electrolyte-interlayer interface. The photocatalytic oxidation of ethanol on TiO2 and TiO 2 modified with Ag and Au nanoparticles was studied by in-situ IR spectroscopy. Au and Ag increased the surface hydroxyl groups, which further served as active species to

  15. Vanadium oxide electrode synthesized by electroless deposition for electrochemical capacitors

    NASA Astrophysics Data System (ADS)

    Wu, Haoran; Lian, Keryn

    2014-12-01

    A thin film vanadium oxide electrode was synthesized by a simple electroless deposition method. Surface and structural analyses revealed that the deposited oxide is a mixture of amorphous V2O5 and VO2. Electrochemical characterizations of the synthesized vanadium oxide showed capacitive behavior with good cycle life. The electroless deposition of vanadium oxide is inexpensive, easy to process, and environmentally benign, offering a promising route for electrode development for electrochemical capacitors.

  16. Electrochemical oxidation of phenol using graphite anodes

    SciTech Connect

    Awad, Y.M.; Abuzaid, N.S.

    1999-02-01

    The effects of current and pH on the electrochemical oxidation of phenol on graphite electrodes is investigated in this study. There was no sign of deterioration of the graphite bed after 5 months of operation. Phenol removal efficiency was a function of the current applied and was around 70% at a current of 2.2 A. The increase of phenol removal efficiency with current is attributed to the increase of ionic transport which increases the rate of electrode reactions responsible for the removal process. The percentage of complete oxidation of phenol increases with current, with a maximum value of about 50%. However, at pH 0.2 it is slightly higher than that at pH 0.5 at all currents. The phenol removal rate increases with increases of current and pH. While the current (CO{sub 2}) efficiency reaches a maximum value in the current range of 1.0--1.2 A, it increases with an increase of acid concentration. The findings of this study have important implications: while anodic oxidation of phenol on graphite can achieve acceptable removal of phenol, the extent of oxidation should not be overlooked.

  17. Graphene oxide sheet-prussian blue nanocomposites: green synthesis and their extraordinary electrochemical properties.

    PubMed

    Liu, Xiao-Wang; Yao, Zi-Jian; Wang, Yue-Feng; Wei, Xian-Wen

    2010-12-01

    A facile and green method for the synthesis of graphene oxide sheets (GOs)-prussian blue nanocomposites has been presented via a spontaneous redox reaction in a aqueous solution containing FeCl3, K3[Fe(CN)6] and graphene oxide sheets. Electrochemical property investigation demonstrates PB nanocubes formed on the surface of GOs retain their excellent electrochemical activity and the GOs can enhance the electron transfer between PB and GC electrode. Moreover, the obtained nanocomposites even have shown a higher sensitivity toward the electrocatalytical reduction of H2O2 than that of multiwalled carbon nanotube/PB nanocomposites. Given their extraordinary electrochemical properties and the green preparation, as-prepared GO-PB nanocomposites have great potential in the field of electrochemical sensor and biofuel cell.

  18. Zirconium Oxide Nanostructures Prepared by Anodic Oxidation

    SciTech Connect

    Dang, Ying Yi; Bhuiyan, Md S; Paranthaman, Mariappan Parans

    2008-01-01

    Zirconium oxide is an advanced ceramic material highly useful for structural and electrical applications because of its high strength, fracture toughness, chemical and thermal stability, and biocompatibility. If highly-ordered porous zirconium oxide membranes can be successfully formed, this will expand its real-world applications, such as further enhancing solid-oxide fuel cell technology. Recent studies have achieved various morphologies of porous zirconium oxide via anodization, but they have yet to create a porous layer where nanoholes are formed in a highly ordered array. In this study, electrochemical methods were used for zirconium oxide synthesis due to its advantages over other coating techniques, and because the thickness and morphology of the ceramic films can be easily tuned by the electrochemical parameters, such as electrolyte solutions and processing conditions, such as pH, voltage, and duration. The effects of additional steps such as pre-annealing and post-annealing were also examined. Results demonstrate the formation of anodic porous zirconium oxide with diverse morphologies, such as sponge-like layers, porous arrays with nanoholes ranging from 40 to 75 nm, and nanotube layers. X-ray powder diffraction analysis indicates a cubic crystallographic structure in the zirconium oxide. It was noted that increased voltage improved the ability of the membrane to stay adhered to the zirconium substrate, whereas lower voltages caused a propensity for the oxide film to flake off. Further studies are needed to define the parameters windows that create these morphologies and to investigate other important characteristics such as ionic conductivity.

  19. ZIRCONIUM OXIDE NANOSTRUCTURES PREPARED BY ANODIC OXIDATION

    SciTech Connect

    Dang, Y. Y.; Bhuiyan, M.S.; Paranthaman, M. P.

    2008-01-01

    Zirconium oxide is an advanced ceramic material highly useful for structural and electrical applications because of its high strength, fracture toughness, chemical and thermal stability, and biocompatibility. If highly-ordered porous zirconium oxide membranes can be successfully formed, this will expand its real-world applications, such as further enhancing solid-oxide fuel cell technology. Recent studies have achieved various morphologies of porous zirconium oxide via anodization, but they have yet to create a porous layer where nanoholes are formed in a highly ordered array. In this study, electrochemical methods were used for zirconium oxide synthesis due to its advantages over other coating techniques, and because the thickness and morphology of the ceramic fi lms can be easily tuned by the electrochemical parameters, such as electrolyte solutions and processing conditions, such as pH, voltage, and duration. The effects of additional steps such as pre-annealing and post-annealing were also examined. Results demonstrate the formation of anodic porous zirconium oxide with diverse morphologies, such as sponge-like layers, porous arrays with nanoholes ranging from 40 to 75 nm, and nanotube layers. X-ray powder diffraction analysis indicates a cubic crystallographic structure in the zirconium oxide. It was noted that increased voltage improved the ability of the membrane to stay adhered to the zirconium substrate, whereas lower voltages caused a propensity for the oxide fi lm to fl ake off. Further studies are needed to defi ne the parameters windows that create these morphologies and to investigate other important characteristics such as ionic conductivity.

  20. Direct electrochemical reduction of graphene oxide on ionic liquid doped screen-printed electrode and its electrochemical biosensing application.

    PubMed

    Ping, Jianfeng; Wang, Yixian; Fan, Kai; Wu, Jian; Ying, Yibin

    2011-10-15

    A novel electrochemical biosensing platform using electrochemically reduced graphene oxide (ER-GNO) modified electrode was proposed. This modified electrode was prepared by one-step electrodeposition of the exfoliated GNO sheets onto the ionic liquid doped screen-printed electrode (IL-SPE). The resulting ER-GNO/IL-SPE brought new capabilities for electrochemical devices by combining the advantages of ER-GNO and disposable electrode. Two important biomolecules, nicotinamide adenine dinucleotide (NADH) and hydrogen peroxide (H(2)O(2)), were employed to study the electrochemical performance of the ER-GNO/IL-SPE, which exhibited more favorable electron transfer kinetics than the bare IL-SPE. On the basis of the greatly enhanced electrochemical reactivity of H(2)O(2) at the developed electrode, ER-GNO and glucose oxidase constructed disposable biosensor showed better analytical performance for the glucose detection compared with the IL-SPE based biosensor. The linear range for the detection of glucose was from 5.0 μM to 12.0 mM with a detection limit of 1.0 μM. This work provides a useful avenue for implementing ER-GNO as a new generation of electrochemical transducer in disposable electrode, which could expand the scope of graphene constructed electrochemical biosensing devices and hold great promise for routine sensing applications.

  1. Preparation of yolk-shell structured copper oxide@silica oxide spheres and their application in high performance electrochemical sensing of Formoterol fumarate residues in swine feed and tissues.

    PubMed

    Gan, Tian; Shi, Zhaoxia; Hu, Danyang; Lv, Zhen; Sun, Junyong; Liu, Yanming

    2016-01-01

    In this paper, we report a facile route to synthesize yolk-shell structured copper oxide@silica oxide (CuO@SiO2) spheres and their application to construct an electrochemical Formoterol fumarate (FF) sensor. The CuO@SiO2 was characterized by means of Fourier transform infrared spectroscopy, X-ray powder diffraction, Raman spectroscopy, scanning electron microscopy, and transmission electron microscopy. Further, FF was electrocatalytically oxidized at the CuO@SiO2 film modified glassy carbon electrode (GCE), which led to a sensitive determination of FF. The oxidation current of FF was linear with concentration in the range of 0.030-10 μM and the detection limit was found to be 5.0 nM (S/N = 3). The observed analytical parameters such as wide linear range, low detection limit and short response time were superior to previously reported FF sensors. Finally, it was demonstrated that the proposed sensor could be used for the selective determination of FF present in swine feed and tissues.

  2. Morphological effects on the electrochemical performance of lithium-rich layered oxide cathodes, prepared by electrospinning technique, for lithium-ion battery applications

    SciTech Connect

    Min, Ji Won; Kalathil, Abdul Kareem; Yim, Chul Jin; Im, Won Bin

    2014-06-01

    Li-rich Li{sub 1.2}Ni{sub 0.17}Co{sub 0.17}Mn{sub 0.5}O{sub 2} cathode materials were synthesized by electrospinning technique with different polymers, and their structural, morphological, and electrochemical performances were investigated. It was found that the electrospinning process leads to the formation of a fiber and flower-like morphology, by using different polymers and heat treatment conditions. The nanostructured morphology provided these materials with high initial discharge capacity. The cycling stability was improved with agglomerated nano-particles, as compared with porous materials. - Highlights: • Fiber and flower-like Li-rich cathode was synthesized by simple electrospinning. • Polymer dependent morphology and electrochemical performance was investigated. • Well-organized porous structure facilitates the diffusion of lithium ions. • Technique could be applicable to other cathode materials as well.

  3. Electrochemical degradation of carbaryl on oxide electrodes.

    PubMed

    Miwa, D W; Malpass, G R P; Machado, S A S; Motheo, A J

    2006-10-01

    This paper presents the study of a prospective electrochemical treatment system for the pesticide carbaryl. Three different dimensionally stable anodes were employed (Ti/Ru0.3 Ti0.7 O2, Ti/Ru0.3 Sn0.7 O2 and Ti/Ir0.3 Ti0.7 O2) and the effect of current density (10, 20, 40 and 60 mA cm(-2)) and supporting electrolyte (0.1 mol L(-1) NaCl and 0.033 mol L(-1) H2SO4) is discussed. All the electrodes present a low level of carbaryl and total organic carbon removal in H2SO4, even at highly positive potentials, indicating that the application of current is not, in itself, sufficient to promote effective oxidation of the pesticide and its products. However, in the presence of NaCl all the electrodes used present rapid diminishing of the carbaryl and total organic carbon content, thus suggesting enhanced activity. The results demonstrate the participation of partially oxidised Cl- species at the electrode surface, which act as an intermediate in the electron transfer between the pesticide molecule and the electrode. Thus, under such conditions, the feasibility of the electrochemical route for the treatment (total or partial) of waste that contains carbaryl is evident.

  4. Mediated electrochemical oxidation of mixed wastes

    SciTech Connect

    Chiba, Z.

    1993-04-01

    The Mediated Electrochemical Oxidation (MEO) process was studied for destroying low-level combustible mixed wastes at Rocky Flats Plant. Tests were performed with non-radioactive surrogate materials: Trimsol for contaminated cutting oils, and reagent-grade cellulose for contaminated cellulosic wastes. Extensive testing was carried out on Trimsol in both small laboratory-scale apparatus and on a large-scale system incorporating an industrial-size electrochemical cell. Preliminary tests were also carried out in the small-scale system with cellulose. Operating and system parameters that were studied were: use of a silver-nitric acid versus a cobalt-sulfuric acid system, effect of electrolyte temperature, effect of acid concentration, and effect of current density. Destruction and coulombic efficiencies were calculated using data obtained from continuous carbon dioxide monitors and total organic carbon (TOC) analysis of electrolyte samples. For Trimsol, the best performance was achieved with the silver-nitrate system at high acid concentrations, temperatures, and current densities. Destruction efficiencies of 99% or greater, and coulombic efficiencies up to 70% were obtained. For the cellulose, high destruction efficiencies and reasonable coulombic efficiencies were obtained for both silver-nitrate and cobalt-sulfate systems.

  5. Electrochemical preparation of hematite nanostructured films for solar hydrogen production

    NASA Astrophysics Data System (ADS)

    Kazemi, N.; Maghsoudipour, A.; Ebadzadeh, T.

    2012-10-01

    Photoelectrochemical water splitting is a clean and promising technique for using a renewable source of energy, i.e., solar energy, to produce hydrogen. In this work electrochemical formation of iron oxyhydroxide and its conversion to hematite (α- Fe2O3) through thermal treatment have been studied. Oxyhydroxide iron compounds have been prepared onto SnO2/F covered glass substrate by potential cycling with two different potential sweep rate values; then calcined at 520 °C in air to obtain α-Fe2O3 nanostrutured films for their implementation as photoanode in a photoelectrochemical cell. X-ray diffraction analysis allowed finding that iron oxides films have nanocrystalline character. Scanning electron microscopy revealed that films have nanostructured morphology. The obtained results are discussed considering the influence of potential sweep rate employed during the preparation of iron oxyhydroxide film on optical, structural and morphological properties of hematite nanostructured films. Results show that films have acceptable characteristics as photoanode in a photoelectrochemical cell for hydrogen generation from water.

  6. Electrochemical oxidation of perfluorinated compounds in water.

    PubMed

    Niu, Junfeng; Li, Yang; Shang, Enxiang; Xu, Zesheng; Liu, Jinzi

    2016-03-01

    Perfluorinated compounds (PFCs) are persistent and refractory organic pollutants that have been detected in various environmental matrices and municipal wastewater. Electrochemical oxidation (EO) is a promising remediation technique for wastewater contaminated with PFCs. A number of recent studies have demonstrated that the "non-active" anodes, including boron-doped diamond, tin oxide, and lead dioxide, are effective in PFCs elimination in wastewater due to their high oxygen evolution potential. Many researchers have conducted experiments to investigate the optimal conditions (i.e., potential, current density, pH value, plate distance, initial PFCs concentration, electrolyte, and other factors) for PFCs elimination to obtain the maximal elimination efficiency and current efficiency. The EO mechanism and pathways of PFCs have been clearly elucidated, which undergo electron transfer, Kolbe decarboxylation or desulfonation, hydrolysis, and radical reaction. In addition, the safety evaluation and energy consumption evaluation of the EO technology have also been summarized to decrease toxic ion release from electrode and reduce the cost of this technique. Although the ultrasonication and hydrothermal techniques combined with the EO process can improve the removal efficiency and current efficiency significantly, these coupled techniques have not been commercialized and applied in industrial wastewater treatment. Finally, key challenges facing EO technology are listed and the directions for further research are pointed out (such as combination with other techniques, treatment for natural waters contaminated by low levels of PFCs, and reactor design).

  7. Oxalic acid mineralization by electrochemical oxidation processes.

    PubMed

    Huang, Yao-Hui; Shih, Yu-Jen; Liu, Cheng-Hong

    2011-04-15

    In this study, two electrochemical oxidation processes were utilized to mineralize oxalic acid which was a major intermediate compound in the oxidation of phenols and other aromatic compounds. The anode rod and cathode net were made of a titanium coated with RuO(2)/IrO(2) (Ti-DSA) and stainless steel (S.S. net, SUS304), respectively. First, the Fered-Fenton process, which used H(2)O(2) and Fe(2+) as additive reagents, achieved 85% of TOC removal. It proceeded with ligand-to-metal charge-transfer (LMCT), which was evidenced by the accumulation of metallic foil on the selected cathode. However, in the absence of H(2)O(2)/Fe(2+), it showed a higher TOC removal efficiency while using Cl(-) only as an additive reagent due to the formation of hypochlorite on the anode. It was also found that the mineralization of oxalic acid by electrolysis generated hypochlorite better than the dosage of commercial hypochlorite without electricity. Also, pH value was a major factor that affected the mineralization efficiency of the oxalic acid due to the chlorine chemistry. 99% TOC removal could be obtained by Cl(-) electrolysis in an acidic environment.

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

    PubMed

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

    2017-02-01

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

  9. Electrode electrolyte interlayers containing cerium oxide for electrochemical fuel cells

    DOEpatents

    Borglum, Brian P.; Bessette, Norman F.

    2000-01-01

    An electrochemical cell is made having a porous fuel electrode (16) and a porous air electrode (13), with solid oxide electrolyte (15) therebetween, where the air electrode surface opposing the electrolyte has a separate, attached, dense, continuous layer (14) of a material containing cerium oxide, and where electrolyte (16) contacts the continuous oxide layer (14), without contacting the air electrode (13).

  10. Oxide modified air electrode surface for high temperature electrochemical cells

    DOEpatents

    Singh, Prabhakar; Ruka, Roswell J.

    1992-01-01

    An electrochemical cell is made having a porous cermet electrode (16) and a porous lanthanum manganite electrode (14), with solid oxide electrolyte (15) between them, where the lanthanum manganite surface next to the electrolyte contains a thin discontinuous layer of high surface area cerium oxide and/or praseodymium oxide, preferably as discrete particles (30) in contact with the air electrode and electrolyte.

  11. Electrochemical water oxidation with carbon-grafted iridium complexes.

    PubMed

    deKrafft, Kathryn E; Wang, Cheng; Xie, Zhigang; Su, Xin; Hinds, Bruce J; Lin, Wenbin

    2012-02-01

    Hydrogen production from water splitting provides a potential solution to storing harvested solar energy in chemical fuels, but this process requires active and robust catalysts that can oxidize water to provide a source of electrons for proton reduction. Here we report the direct, covalent grafting of molecular Ir complexes onto carbon electrodes, with up to a monolayer coverage. Carbon-grafted Ir complexes electrochemically oxidize water with a turnover frequency of up to 3.3 s(-1) and a turnover number of 644 during the first hour. Electrochemical water oxidation with grafted catalysts gave enhanced rates and stability compared to chemically driven water oxidation with the corresponding molecular catalysts. This strategy provides a way to systematically evaluate catalysts under tunable conditions, potentially providing new insights into electrochemical water oxidation processes and water oxidation catalyst design.

  12. Hydrothermal preparation and electrochemical sensing properties of TiO(2)-graphene nanocomposite.

    PubMed

    Fan, Yang; Lu, Hai-Ting; Liu, Jin-Hang; Yang, Chun-Peng; Jing, Qiang-Shan; Zhang, Yu-Xia; Yang, Xing-Kun; Huang, Ke-Jing

    2011-03-01

    A facile hydrothermal method has been developed and shown to be effective for the preparation of TiO(2)-graphene nanocomposite. The as-prepared nanocomposite was characterized using FT-IR spectroscopy, powder X-ray diffraction (XRD) and scanning electron microscopy (SEM). The TiO(2)-graphene modified glassy carbon electrode (GCE) exhibited remarkable electron transfer kinetics and electrocatalytic activity toward the oxidation of dopamine (DA). Furthermore, the oxidation of common interfering agent such as ascorbic acid (AA) was significantly suppressed at this modified electrode, which resulted in good selectivity and sensitivity for electrochemical sensing of DA. These results demonstrate that the TiO(2)-graphene hybrid material has promising potential applications in electrochemical sensors and biosensors design.

  13. Innovative oxide materials for electrochemical energy conversion

    NASA Astrophysics Data System (ADS)

    Wachsman, Eric D.

    2012-02-01

    Research in functional materials has progressed from those materials exhibiting structural to electronic functionality. The study of ion conducting ceramics ushers in a new era of ``chemically functional materials.'' This chemical functionality arises out of the defect equilibria of these materials, and results in the ability to transport chemical species and actively participate in chemical reactions at their surface. Moreover, this chemical functionality provides a promise for the future whereby the harnessing of our natural hydrocarbon energy resources can shift from inefficient and polluting combustion - mechanical methods to direct electrochemical conversion. The unique properties of these materials and their applications will be described. The focus will be on the application of ion conducting ceramics to energy conversion and storage, chemical sensors, chemical separation and conversion, and life support systems. Results presented will include development of record high power density (3 kW/kg) solid oxide fuel cells, NOx/CO species selective solid-state sensors, high yield membrane reactors, and regenerative life support systems that reduce CO2 to O2 and solid C.

  14. Solution synthesis of metal oxides for electrochemical energy storage applications.

    PubMed

    Xia, Xinhui; Zhang, Yongqi; Chao, Dongliang; Guan, Cao; Zhang, Yijun; Li, Lu; Ge, Xiang; Bacho, Ignacio Mínguez; Tu, Jiangping; Fan, Hong Jin

    2014-05-21

    This article provides an overview of solution-based methods for the controllable synthesis of metal oxides and their applications for electrochemical energy storage. Typical solution synthesis strategies are summarized and the detailed chemical reactions are elaborated for several common nanostructured transition metal oxides and their composites. The merits and demerits of these synthesis methods and some important considerations are discussed in association with their electrochemical performance. We also propose the basic guideline for designing advanced nanostructure electrode materials, and the future research trend in the development of high power and energy density electrochemical energy storage devices.

  15. Preparation and electrochemical properties of core-shell carbon coated Mn-Sn complex metal oxide as anode materials for lithium-ion batteries

    NASA Astrophysics Data System (ADS)

    Zhang, Ruixue; Fang, Guoqing; Liu, Weiwei; Xia, Bingbo; Sun, Hongdan; Zheng, Junwei; Li, Decheng

    2014-02-01

    In this study, we synthesized a carbon coated Mn-Sn metal oxide composite with core-shell structure (MTO@C) via a simple glucose hydrothermal reaction and subsequent carbonization approach. When the MTO@C composite was applied as an anode material for lithium-ion batteries, it maintained a reversible capacity of 409 mA h g-1 after 200 cycles at a current density of 100 mA g-1. The uniformed and continuous carbon layer formed on the MTO nanoparticles, effectively buffered the volumetric change of the active material and increased electronic conductivity, which thus prolonged the cycling performance of the MTO@C electrode.

  16. Porous nickel oxide films for electrochemical capacitors

    SciTech Connect

    Liu, K.C.; Anderson, M.A.

    1995-12-31

    NiO/Ni composite thin films consisting of nano-sized particles have been found to perform as good electrodes in electrochemical capacitor applications. These films can provide a specific capacitance of 25--40 F/g. The low cost of raw materials and easy manufacturing process of this system should allow one to produce low-cost electrochemical capacitors.

  17. PREPARATION OF REFRACTORY OXIDE MICROSPHERE

    DOEpatents

    Haws, C.C. Jr.

    1963-09-24

    A method is described of preparing thorium oxide in the form of fused spherical particles about 1 to 2 microns in diameter. A combustible organic solution of thorium nitrate containing additive metal values is dispersed into a reflected, oxygen-fed flame at a temperature above the melting point of the resulting oxide. The metal additive is aluminum at a proportion such as to provide 1 to 10 weight per cent aluminum oxide in the product, silicon at the same proportion, or beryllium at a proportion of 12 to 25 weight per cent beryllium oxide in the product. A minor proportion of uranium values may also be provided in the solution. The metal additive lowers the oxide melting point and allows fusion and sphere formation in conventional equipment. The product particles are suitable for use in thorium oxide slurries for nuclear reactors. (AEC)

  18. Preparation of tungsten oxide

    DOEpatents

    Bulian, Christopher J.; Dye, Robert C.; Son, Steven F.; Jorgensen, Betty S.; Perry, W. Lee

    2009-09-22

    Tungsten trioxide hydrate (WO.sub.3.H.sub.2O) was prepared from a precursor solution of ammonium paratungstate in concentrated aqueous hydrochloric acid. The precursor solution was rapidly added to water, resulting in the crash precipitation of a yellow white powder identified as WO.sub.3.H.sub.2O nanosized platelets by x-ray diffraction and scanning electron microscopy. Annealing of the powder at 200.degree. C. provided cubic phase WO.sub.3 nanopowder, and at 400.degree. C. provided WO.sub.3 nanopowder as a mixture of monoclinic and orthorhombic phases.

  19. Electrochemical and partial oxidation of methane

    NASA Astrophysics Data System (ADS)

    Singh, Rahul

    2008-10-01

    Hydrogen has been the most common fuel used for the fuel cell research but there remains challenging technological hurdles and storage issues with hydrogen fuel. The direct electrochemical oxidation of CH4 (a major component of natural gas) in a solid oxide fuel cell (SOFC) to generate electricity has a potential of commercialization in the area of auxiliary and portable power units and battery chargers. They offer significant advantages over an external reformer based SOFC, namely, (i) simplicity in the overall system architecture and balance of plant, (ii) more efficient and (iii) availability of constant concentration of fuel in the anode compartment of SOFC providing stability factor. The extreme operational temperature of a SOFC at 700-1000°C provides a thermodynamically favorable pathway to deposit carbon on the most commonly used Ni anode from CH4 according to the following reaction (CH4 = C + 2H2), thus deteriorating the cell performance, stability and durability. The coking problem on the anode has been a serious and challenging issue faced by the catalyst research community worldwide. This dissertation presents (i) a novel fabricated bi-metallic Cu-Ni anode by electroless plating of Cu on Ni anode demonstrating significantly reduced or negligible coke deposition on the anode for CH4 and natural gas fuel after long term exposure, (ii) a thorough microstructural examination of Ni and Cu-Ni anode exposed to H2, CH4 and natural gas after long term exposure at 750°C by scanning electron microscopy, energy dispersive X-ray spectroscopy and X-ray diffraction and (iii) in situ electrochemical analysis of Ni and Cu-Ni for H2, CH4 and natural gas during long term exposure at 750°C by impedance spectroscopy. A careful investigation of variation in the microstructure and performance characteristics (voltage-current curve and impedance) of Ni and Cu-Ni anode before and after a long term exposure of CH4 and natural gas would allow us to test the validation of a

  20. Physical and electrochemical study of cobalt oxide nano- and microparticles

    SciTech Connect

    Alburquenque, D.; Vargas, E.; Denardin, J.C.; Escrig, J.; Marco, J.F.; Gautier, J.L.

    2014-07-01

    Cobalt oxide nanocrystals of size 17–21 nm were synthesized by a simple reaction between cobalt acetate (II) and dodecylamine. On the other hand, micrometric Co{sub 3}O{sub 4} was prepared using the ceramic method. The structural examination of these materials was performed using powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and transmission electron microscopy (TEM and HRTEM). XRD studies showed that the oxides were pure, well-crystallized, spinel cubic phases with a-cell parameter of 0.8049 nm and 0.8069 nm for the nano and micro-oxide, respectively. The average particle size was 19 nm (nano-oxide) and 1250 μm (micro-oxide). Morphological studies carried out by SEM and TEM analyses have shown the presence of octahedral particles in both cases. Bulk and surface properties investigated by X-ray photoelectron spectroscopy (XPS), point zero charge (pzc), FTIR and cyclic voltammetry indicated that there were no significant differences in the composition on both materials. The magnetic behavior of the samples was determined using a vibrating sample magnetometer. The compounds showed paramagnetic character and no coercivity and remanence in all cases. Galvanostatic measurements of electrodes formed with nanocrystals showed better performance than those built with micrometric particles. - Highlights: • Spinel Co{sub 3}O{sub 4} nanoparticles and microparticles with same structure but with different cell parameters, particle size and surface area were synthesized. • Oxide nanoparticles showed better electrochemical behavior than micrometric ones due to area effect.

  1. Electrochemical preparation of carbon chains and nanoparticles

    NASA Astrophysics Data System (ADS)

    Kavan, Ladislav

    1999-09-01

    The composite of carbon with alkali metal fluoride, C-MF(M=Li, Na) was prepared by cathodic defluorination of perfluorinated hydrocarbons at room temperature. Raman spectra of C-MF from PTFE indicate carbon chains (oligoynes, 1974-2024 cm-1) in addition to graphite-like carbon (1300-1500 cm-1). The oligoyne-containing carbon is partly selforganized by cross linking towards graphene. Highly-organized carbons were prepared from friction-deposited PTFE films. AFM confirms perfect ordering of the precursor molecules (up to atomic resolution), but the corresponding carbonization product is rapidly reconstructed upon contact to air. Raman spectra of oriented carbons display high conjugation lengths (up to 18 sp-bonded carbon atoms). Cyclic perfluorinated precursors are also smoothly defluorinated to elemental carbon. TEM indicates that these carbons contain about 1% of carbonaceous nanoparticles, i.e. nanotubes and onions. Also small quantity of fullerene C60(≈0.01%) was detected in the toluene extract.

  2. PREPARATION OF REFRACTORY OXIDE CRYSTALS

    DOEpatents

    Grimes, W.R.; Shaffer, J.H.; Watson, G.M.

    1962-11-13

    A method is given for preparing uranium dioxide, thorium oxide, and beryllium oxide in the form of enlarged individual crystals. The surface of a fused alkali metal halide melt containing dissolved uranium, thorium, or beryllium values is contacted with a water-vapor-bearing inert gas stream at a rate of 5 to 10 cubic centimeters per minute per square centimeter of melt surface area. Growth of individual crystals is obtained by prolonged contact. Beryllium oxide-coated uranium dioxide crystals are prepared by disposing uranium dioxide crystals 5 to 20 microns in diameter in a beryllium-containing melt and contacting the melt with a water-vapor-bearing inert gas stream in the same manner. (AEC)

  3. High Power Electrochemical Capacitors

    DTIC Science & Technology

    2012-03-23

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

  4. Electrochemical slurry compositions and methods for preparing the same

    SciTech Connect

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

    2016-11-01

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

  5. In Situ Electrochemical Oxidation Tuning of Transition Metal Disulfides to Oxides for Enhanced Water Oxidation

    PubMed Central

    2015-01-01

    The development of catalysts with earth-abundant elements for efficient oxygen evolution reactions is of paramount significance for clean and sustainable energy storage and conversion devices. Our group demonstrated recently that the electrochemical tuning of catalysts via lithium insertion and extraction has emerged as a powerful approach to improve catalytic activity. Here we report a novel in situ electrochemical oxidation tuning approach to develop a series of binary, ternary, and quaternary transition metal (e.g., Co, Ni, Fe) oxides from their corresponding sulfides as highly active catalysts for much enhanced water oxidation. The electrochemically tuned cobalt–nickel–iron oxides grown directly on the three-dimensional carbon fiber electrodes exhibit a low overpotential of 232 mV at current density of 10 mA cm–2, small Tafel slope of 37.6 mV dec–1, and exceptional long-term stability of electrolysis for over 100 h in 1 M KOH alkaline medium, superior to most non-noble oxygen evolution catalysts reported so far. The materials evolution associated with the electrochemical oxidation tuning is systematically investigated by various characterizations, manifesting that the improved activities are attributed to the significant grain size reduction and increase of surface area and electroactive sites. This work provides a promising strategy to develop electrocatalysts for large-scale water-splitting systems and many other applications. PMID:27162978

  6. In Situ Electrochemical Oxidation Tuning of Transition Metal Disulfides to Oxides for Enhanced Water Oxidation

    DOE PAGES

    Chen, Wei; Wang, Haotian; Li, Yuzhang; ...

    2015-07-15

    The development of catalysts with earth-abundant elements for efficient oxygen evolution reactions is of paramount significance for clean and sustainable energy storage and conversion devices. Our group demonstrated recently that the electrochemical tuning of catalysts via lithium insertion and extraction has emerged as a powerful approach to improve catalytic activity. Here we report a novel in situ electrochemical oxidation tuning approach to develop a series of binary, ternary, and quaternary transition metal (e.g., Co, Ni, Fe) oxides from their corresponding sulfides as highly active catalysts for much enhanced water oxidation. The electrochemically tuned cobalt–nickel–iron oxides grown directly on the three-dimensionalmore » carbon fiber electrodes exhibit a low overpotential of 232 mV at current density of 10 mA cm–2, small Tafel slope of 37.6 mV dec–1, and exceptional long-term stability of electrolysis for over 100 h in 1 M KOH alkaline medium, superior to most non-noble oxygen evolution catalysts reported so far. The materials evolution associated with the electrochemical oxidation tuning is systematically investigated by various characterizations, manifesting that the improved activities are attributed to the significant grain size reduction and increase of surface area and electroactive sites. This work provides a promising strategy to develop electrocatalysts for large-scale water-splitting systems and many other applications.« less

  7. [Research on synergy of combining electrochemical oxidation and catalytic wet oxidation].

    PubMed

    Wang, Hua; Li, Guang-Ming; Zhang, Fang; Huang, Ju-Wen

    2009-07-15

    A new catalytic wet oxidation fixed-bed reactor combined with three-dimensional electric-field was developed to investigate catalytic wet oxidation, electrochemical oxidation and electroassisted catalytic wet oxidation of the solution containing phenol in the presence of a catalyst Mn-Sn-Sb-3/gamma-Al2O3. Good electroassisted catalytic wet oxidation efficiency was obtained in the setup for the combination system even at mild conditions (T = 130 degrees C, po2 = 1.0 MPa) that the phenol conversion and TOC reduction were up to 94.0% and 88.4% after 27 min treatment, respectively. The result also shows that the rate constants of electroassisted catalytic wet oxidation are much higher than that of not only both catalytic wet oxidation and electrochemical oxidation process alone but also additive efficiencies of catalytic wet oxidation and electrochemical oxidation processes, which indicates an apparent synergetic effect between CWO and ECO processes.

  8. Alkaline electrochemical advanced oxidation process for chromium oxidation at graphitized multi-walled carbon nanotubes.

    PubMed

    Xue, Yudong; Zheng, Shili; Sun, Zhi; Zhang, Yi; Jin, Wei

    2017-09-01

    Alkaline electrochemical advanced oxidation processes for chromium oxidation and Cr-contaminated waste disposal were reported in this study. The highly graphitized multi-walled carbon nanotubes g-MWCNTs modified electrode was prepared for the in-situ electrochemical generation of HO2(-). RRDE test results illustrated that g-MWCNTs exhibited much higher two-electron oxygen reduction activity than other nanocarbon materials with peak current density of 1.24 mA cm(-2), %HO2(-) of 77.0% and onset potential of -0.15 V (vs. Hg/HgO). It was originated from the highly graphitized structure and good electrical conductivity as illustrated from the Raman, XRD and EIS characterizations, respectively. Large amount of reactive oxygen species (HO2(-) and ·OH) were in-situ electro-generated from the two-electron oxygen reduction and chromium-induced alkaline electro-Fenton-like reaction. The oxidation of Cr(III) was efficiently achieved within 90 min and the conversion ratio maintained more than 95% of the original value after stability test, offering an efficient and green approach for the utilization of Cr-containing wastes. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

    PubMed

    Mai, Yiyong; Zhang, Fan; Feng, Xinliang

    2014-01-07

    Metal oxide-containing nanomaterials (MOCNMs) of controllable structures at the nano-scale have attracted considerable interest because of their great potential applications in electrochemical energy storage devices, such as lithium-ion batteries (LIBs) and supercapacitors. Among many structure-directing agents, polymers and macromolecules, including block copolymers (BCPs) and graphene, exhibit distinct advantages in the template-assisted synthesis of MOCNMs. In this feature article, we introduce the controlled preparation of MOCNMs employing BCPs and graphene as structure-directing agents. Typical synthetic strategies are presented for the control of structures and sizes as well as the improvement of physical properties and electrochemical performance of MOCNMs in LIBs and supercapacitors.

  10. DEVELOPMENT OF ELECTROCHEMICAL REDUCTION TECHNOLOGY FOR SPENT OXIDE FUELS

    SciTech Connect

    Hur, Jin-Mok; Seo, Chung-Seok; Kim, Ik-Soo; Hong, Sun-Seok; Kang, Dae-Seung; Park, Seong-Won

    2003-02-27

    The Advanced Spent Fuel Conditioning Process (ACP) has been under development at Korea Atomic Energy Research Institute (KAERI) since 1997. The concept is to convert spent oxide fuel into metallic form and to remove high heat-load fission products such as Cs and Sr from the spent fuel. The heat power, volume, and radioactivity of spent fuel can decrease by a factor of a quarter via this process. For the realization of ACP, a concept of electrochemical reduction of spent oxide fuel in Li2O-LiCl molten salt was proposed and several cold tests using fresh uranium oxides have been carried out. In this new electrochemical reduction process, electrolysis of Li2O and reduction of uranium oxide are taking place simultaneously at the cathode part of electrolysis cell. The conversion of uranium oxide to uranium metal can reach more than 99% ensuring the feasibility of this process.

  11. Method of preparing a positive electrode for an electrochemical cell

    DOEpatents

    Tomczuk, Zygmunt

    1979-01-01

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

  12. Electrochemical study of DNA damaged by oxidation stress.

    PubMed

    Zitka, Ondrej; Krizkova, Sona; Skalickova, Sylvie; Kopel, Pavel; Babula, Petr; Adam, Vojtech; Kizek, Rene

    2013-02-01

    Many compounds can interact with DNA leading to changes of DNA structure as point mutation and bases excision, which could trigger some metabolic failures, which leads to the changes in DNA structure resulting in cancer. Oxidation of nucleic acid bases belongs to the one of the mostly occurred type of DNA damaging leading to the above mentioned phenomena. The investigation of processes of DNA oxidation damage is topical and electrochemical methods include a versatile and sensitive tool for these purposes. 8-hydroxydeoxyguanosine (8-OHdG) is the most widely accepted marker of DNA damage. Oxidative damage to DNA by free radicals and exposure to ionizing radiation generate several other products within the double helix besides mentioned oxidation products of nucleic acid bases. The basic electrochemical behaviour of nucleic acids bases on various types of carbon electrodes is reviewed. Further, we address our attention on description of oxidation mechanisms and on detection of the most important products of nucleic bases oxidation. The miniaturization of detector coupled with some microfluidic devices is suggested and discussed. The main aim of this review is to report the advantages and features of the electrochemical detection of guanine oxidation product as 8-OHdG and other similarly produced molecules as markers for DNA damage.

  13. Treatment of Radioactive Organic Wastes by an Electrochemical Oxidation

    SciTech Connect

    Kim, K.H.; Ryue, Y.G.; Kwak, K.K.; Hong, K.P.; Kim, D.H.

    2007-07-01

    A waste treatment system by using an electrochemical oxidation (MEO, Mediated Electrochemical Oxidation) was installed at KAERI (Korea Atomic Energy Research Institute) for the treatment of radioactive organic wastes, especially EDTA (Ethylene Diamine Tetraacetic Acid) generated during the decontamination activity of nuclear installations. A cerium and silver mediated electrochemical oxidation technique method has been developed as an alternative for an incineration process. An experiment to evaluate the applicability of the above two processes and to establish the conditions to operate the pilot-scale system has been carried out by changing the concentration of the catalyst and EDTA, the operational current density, the operating temperature, and the electrolyte concentration. As for the results, silver mediated oxidation was more effective in destructing the EDTA wastes than the cerium mediated oxidation process. For a constant volume of the EDTA wastes, the treatment time for the cerium-mediated oxidation was 9 hours and its conversion ratio of EDTA to water and CO{sub 2} was 90.2 % at 80 deg. C, 10 A, but the treatment time for the silver-mediated oxidation was 3 hours and its conversion ratio was 89.2 % at 30 deg. C, 10 A. (authors)

  14. Corrosion and Electrochemical Oxidation of a Pyrite by Thiobacillus ferrooxidans

    PubMed Central

    Mustin, C.; Berthelin, J.; Marion, P.; de Donato, P.

    1992-01-01

    The oxidation of a pure pyrite by Thiobacillus ferrooxidans is not really a constant phenomenon; it must be considered to be more like a succession of different steps which need characterization. Electrochemical studies using a combination of a platinum electrode and a specific pyrite electrode (packed-ground-pyrite electrode) revealed four steps in the bioleaching process. Each step can be identified by the electrochemical behavior (redox potentials) of pyrite, which in turn can be related to chemical (leachate content), bacterial (growth), and physical (corrosion patterns) parameters of the leaching process. A comparison of the oxidation rates of iron and sulfur indicated the nonstoichiometric bacterial oxidation of a pure pyrite in which superficial phenomena, aqueous oxidation, and deep crystal dissolution are successively involved. Images PMID:16348688

  15. High Temperature Oxidation and Electrochemical Studies Related to Hot Corrosion

    DTIC Science & Technology

    1989-12-01

    thin film of liquid sodium sulfate. It appears that the initial formation of metal oxides is necessary for the initial reaction and the transport of...compounds in the silica film allow transport of alkali metal cations under an electrochemical driving force with essentially no electronic conduction

  16. Electrochemical advanced oxidation processes: today and tomorrow. A review.

    PubMed

    Sirés, Ignasi; Brillas, Enric; Oturan, Mehmet A; Rodrigo, Manuel A; Panizza, Marco

    2014-01-01

    In recent years, new advanced oxidation processes based on the electrochemical technology, the so-called electrochemical advanced oxidation processes (EAOPs), have been developed for the prevention and remediation of environmental pollution, especially focusing on water streams. These methods are based on the electrochemical generation of a very powerful oxidizing agent, such as the hydroxyl radical ((•)OH) in solution, which is then able to destroy organics up to their mineralization. EAOPs include heterogeneous processes like anodic oxidation and photoelectrocatalysis methods, in which (•)OH are generated at the anode surface either electrochemically or photochemically, and homogeneous processes like electro-Fenton, photoelectro-Fenton, and sonoelectrolysis, in which (•)OH are produced in the bulk solution. This paper presents a general overview of the application of EAOPs on the removal of aqueous organic pollutants, first reviewing the most recent works and then looking to the future. A global perspective on the fundamentals and experimental setups is offered, and laboratory-scale and pilot-scale experiments are examined and discussed.

  17. Preparation and electrochemical properties of urchin-like La0.8Sr0.2MnO3 perovskite oxide as a bifunctional catalyst for oxygen reduction and oxygen evolution reaction

    NASA Astrophysics Data System (ADS)

    Jin, Chao; Cao, Xuecheng; Zhang, Liya; Zhang, Cong; Yang, Ruizhi

    2013-11-01

    An urchin-like La0.8Sr0.2MnO3 (LSM) perovskite oxide has been synthesized through a co-precipitation method with urea as a precipitator, and characterized by thermogravimetric analysis (TGA), X-ray diffraction (XRD), scanning electron microscopy (SEM) and BET analysis. SEM results show that a micro/nanocomposite with an urchin-like morphology has been obtained. The as-synthesized LSM perovskite oxide has a high specific surface area of 48 m2 g-1. The catalytic activity of the oxide for the oxygen reduction reaction (ORR) and the oxygen evolution reaction (OER) in 0.1 M KOH solution has been studied by using a rotating-ring-disk electrode (RRDE). In the ORR test, a maximum cathodic current density of 5.2 mA cm-2 at -1.0 V (vs. Ag/AgCl) with 2500 rpm was obtained, and the ORR mainly favors a direct four-electron pathway. The results of anodic linear scanning voltammograms indicate that the urchin-like LSM perovskite oxide exhibits an encouraging catalytic activity for the OER. All electrochemical measurements suggest that the urchin-like LSM perovskite oxide could be used as a bifunctional catalyst for the ORR and the OER.

  18. Electrochemical oxidation of imazapyr with BDD electrode in titanium substrate.

    PubMed

    Souza, F L; Teodoro, T Q; Vasconcelos, V M; Migliorini, F L; Lima Gomes, P C F; Ferreira, N G; Baldan, M R; Haiduke, R L A; Lanza, M R V

    2014-12-01

    In this work we have studied the treatment of imazapyr by electrochemical oxidation with boron-doped diamond anode. Electrochemical degradation experiments were performed in a one-compartment cell containing 0.45 L of commercial formulations of herbicide in the pH range 3.0-10.0 by applying a density current between 10 and 150 mA cm(-2) and in the temperature range 25-45 °C. The maximum current efficiencies were obtained at lower current densities since the electrochemical system is under mass transfer control. The mineralization rate increased in acid medium and at higher temperatures. The treatment was able to completely degrade imazapyr in the range 4.6-100.0 mg L(-1), although the current charge required rises along with the increasing initial concentration of the herbicide. Toxicity analysis with the bioluminescent bacterium Vibrio fischeri showed that at higher pollutant concentrations the toxicity was reduced after the electrochemical treatment. To clarify the reaction pathway for imazapyr mineralization by OH radicals, LC-MS/MS analyses we performed together with a theoretical study. Ions analysis showed the formation of high levels of ammonium in the cathode. The main final products of the electrochemical oxidation of imazapyr with diamond thin film electrodes are formic, acetic and butyric acids.

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

    DOEpatents

    Bandyopadhyay, Gautam; Dusek, Joseph T.

    1981-01-01

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

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

    DOEpatents

    Bandyopadhyay, G.; Dusek, J.T.

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

  1. Method of electrode fabrication for solid oxide electrochemical cells

    DOEpatents

    Jensen, Russell R.

    1990-01-01

    A process for fabricating cermet electrodes for solid oxide electrochemical cells by sintering is disclosed. First, a porous metal electrode is fabricated on a solid oxide cell, such as a fuel cell by, for example, sintering, and is then infiltrated with a high volume fraction stabilized zirconia suspension. A second sintering step is used to sinter the infiltrated zirconia to a high density in order to more securely attach the electrode to the solid oxide electrolyte of the cell. High performance fuel electrodes can be obtained with this process. Further electrode performance enhancement may be achieved if stabilized zirconia doped with cerium oxide, chromium oxide, titanium oxide, and/or praseodymium oxide for electronic conduction is used.

  2. Method of electrode fabrication for solid oxide electrochemical cells

    DOEpatents

    Jensen, R.R.

    1990-11-20

    A process for fabricating cermet electrodes for solid oxide electrochemical cells by sintering is disclosed. First, a porous metal electrode is fabricated on a solid oxide cell, such as a fuel cell by, for example, sintering, and is then infiltrated with a high volume fraction stabilized zirconia suspension. A second sintering step is used to sinter the infiltrated zirconia to a high density in order to more securely attach the electrode to the solid oxide electrolyte of the cell. High performance fuel electrodes can be obtained with this process. Further electrode performance enhancement may be achieved if stabilized zirconia doped with cerium oxide, chromium oxide, titanium oxide, and/or praseodymium oxide for electronic conduction is used. 5 figs.

  3. Chitosan/graphene oxide nanocomposite films with enhanced interfacial interaction and their electrochemical applications

    NASA Astrophysics Data System (ADS)

    He, Linghao; Wang, Hongfang; Xia, Guangmei; Sun, Jing; Song, Rui

    2014-09-01

    A series of chitosan (CS) nanocomposites incorporated with graphene oxide (GO) nanosheets were facilely prepared by sonochemical method. Characterized by scanning electron microscopy, the obtained nanocomposites showed fine dispersion of GO in the CS matrix. Meanwhile, a marked interfacial interaction was also revealed as the values of glass transition temperature, the decomposition temperature and the storage modulus were significantly increased with the addition of GO. Furthermore, the well dispersed GO nanosheets could significantly improve the electrochemical activity of the CS as demonstrated by the electrochemical behaviors of pure CS and the GO/CS composite electrodes. Hence, the GO/CS nanocomposites film could be a promising candidate in the fabrication of electrochemical biosensors.

  4. Zinc oxide nanostructures for electrochemical cortisol biosensing

    NASA Astrophysics Data System (ADS)

    Vabbina, Phani Kiran; Kaushik, Ajeet; Tracy, Kathryn; Bhansali, Shekhar; Pala, Nezih

    2014-05-01

    In this paper, we report on fabrication of a label free, highly sensitive and selective electrochemical cortisol immunosensors using one dimensional (1D) ZnO nanorods (ZnO-NRs) and two dimensional nanoflakes (ZnO-NFs) as immobilizing matrix. The synthesized ZnO nanostructures (NSs) were characterized using scanning electron microscopy (SEM), selective area diffraction (SAED) and photoluminescence spectra (PL) which showed that both ZnO-NRs and ZnO-NFs are single crystalline and oriented in [0001] direction. Anti-cortisol antibody (Anti-Cab) are used as primary capture antibodies to detect cortisol using electrochemical impedance spectroscopy (EIS). The charge transfer resistance increases linearly with increase in cortisol concentration and exhibits a sensitivity of 3.078 KΩ. M-1 for ZnO-NRs and 540 Ω. M -1 for ZnO-NFs. The developed ZnO-NSs based immunosensor is capable of detecting cortisol at 1 pM. The observed sensing parameters are in physiological range. The developed sensors can be integrated with microfluidic system and miniaturized potentiostat to detect cortisol at point-of-care.

  5. Method of preparing an electrochemical cell in uncharged state

    DOEpatents

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

    1977-02-01

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

  6. Cobalt vanadium oxide thin nanoplates: primary electrochemical capacitor application

    PubMed Central

    Zhang, Youjuan; Liu, Yuanying; Chen, Jing; Guo, Qifei; Wang, Ting; Pang, Huan

    2014-01-01

    Co3V2O8 thin nanoplates are firstly described as a kind of electrode material for supercapacitors. More importantly, from electrochemical measurements, the obtained Co3V2O8 nanoplate electrode shows a good specific capacitance (0.5 A g−1, 739 F g−1) and cycling stability (704 F g−1 retained after 2000 cycles). This study essentially offers a new kind of metal vanadium oxides as electrochemical active material for the development of supercapacitors. PMID:25023373

  7. Development of a facile and effective electrochemical strategy for preparation of iron oxides (Fe3O4 and γ-Fe2O3) nanoparticles from aqueous and ethanol mediums and in situ PVC coating of Fe3O4 superparamagnetic nanoparticles for biomedical applications

    NASA Astrophysics Data System (ADS)

    Karimzadeh, Isa; Dizaji, Hamid Rezagholipour; Aghazadeh, Mustafa

    2016-10-01

    To attain reliable and high performance in biomedical applications, magnetic particles with regular spherical shape, narrow size distributions, high-saturation magnetization, and good dispersion in liquid media is very important. Therefore, the synthesis of monodispersed, water-dispersible, and regular spherical superparamagnetic iron oxides nanoparticles (SPIONs) with high saturation magnetization will be of great importance. Here we report a facile, fact and simple electrochemical tactic for preparation of SPIONs and their one step in situ surface engineering in both aqueous and ethanol mediums. In this platform, optimum and simple electrochemical conditions were first constructed for preparation of Fe3O4 and γ-Fe2O3 nanoparticles in both ethanol and aqueous mediums, and monodispersed nanoparticles with superparamagnetic properties were prepared. The field emission scanning and transmission electron microscopy (FE-SEM and TEM) observations revealed that the electrodeposited nanoparticles have roughly spherical and homogeneous shape with narrow size distribution. Then, Fe3O4 nanoparticles were coated by polyvinyl chloride (PVC) during deposition process. The PVC coating on SPIONs surface was confirmed by Fourier transform infrared spectroscopy (FT-IR), dynamic light scattering (DLS), differential scanning calorimetry (DSC), and thermogravimetric (TG) analyses. Results of vibrating sample magnetometer (VSM) indicated that the prepared SPIONs exhibit superparamagnetic behavior including negligible remnant magnetization and negligible coercivity, and high saturation magnetization at room temperature. PVC coated SPIONs exhibited saturation magnetization value of 43.72 emu/g, and negligible remnant magnetization and coercivity (Mr~0.15 emu/g and Ce~0.5 Oe, respectively). Based on the obtained results, it was concluded this electrochemical strategy can be introduced as a novel and clean platform for preparation of variety polymer and drug coated/loaded SPIONs for

  8. Noncovalent attachment of NAD+ cofactor onto carbon nanotubes for preparation of integrated dehydrogenase-based electrochemical biosensors.

    PubMed

    Zhou, Haojie; Zhang, Zipin; Yu, Ping; Su, Lei; Ohsaka, Takeo; Mao, Lanqun

    2010-04-20

    This study describes a facile approach to the preparation of integrated dehydrogenase-based electrochemical biosensors through noncovalent attachment of an oxidized form of beta-nicotinamide adenine dinucleotide (NAD(+)) onto carbon nanotubes with the interaction between the adenine subunit in NAD(+) molecules and multiwalled carbon nanotubes (MWCNTs). X-ray photoelectron spectroscopic and cyclic voltammetric results suggest that NAD(+) is noncovalently attached onto MWCNTs to form an NAD(+)/MWCNT composite that acts as the electronic transducer for the integrated dehydrogenase-based electrochemical biosensors. With glucose dehydrogenase (GDH) as a model dehydrogenase-based recognition unit, electrochemical studies reveal that glucose is readily oxidized at the GDH/NAD(+)/MWCNT-modified electrode without addition of NAD(+) in the phosphate buffer. The potential for the oxidation of glucose at the GDH/NAD(+)/MWCNT-modified electrode remains very close to that for NADH oxidation at the MWCNT-modified electrode, but it is more negative than those for the oxidation of glucose at the MWCNT-modified electrode and for NADH oxidation at a bare glassy carbon electrode. These results demonstrate that NAD(+) molecules stably attached onto MWCNTs efficiently act as the cofactor for the dehydrogenases. MWCNTs employed here not only serve as the electronic transducer and the support to confine NAD(+) cofactor onto the electrode surface, but also act as the electrocatalyst for NADH oxidation in the dehydrogenase-based electrochemical biosensors. At the GDH/NAD(+)/MWCNT-based glucose biosensor, the current is linear with the concentration of glucose being within a concentration range from 10 to 300 microM with a limit of detection down to 4.81 microM (S/N = 3). This study offers a facile and versatile approach to the development of integrated dehydrogenase-based electrochemical devices, such as electrochemical biosensors and biofuel cells.

  9. Electrochemically Exfoliated Graphene and Graphene Oxide for Energy Storage and Electrochemistry Applications.

    PubMed

    Ambrosi, Adriano; Pumera, Martin

    2016-01-04

    Top-down methods are of key importance for large-scale graphene and graphene oxide preparation. Electrochemical exfoliation of graphite has lately gained much interest because of the simplicity of execution, the short process time, and the good quality of graphene that can be obtained. Here, we test three different electrolytes, that is, H2 SO4 , Na2 SO4 , and LiClO4 , with a common exfoliation procedure to evaluate the difference in structural and chemical properties that result for the graphene. The properties are analyzed by means of scanning transmission electron microscopy (STEM), Raman spectroscopy, and X-ray photoelectron spectroscopy. We then tested the graphene materials for electrochemical applications, measuring the heterogeneous electron transfer (HET) rates with a Fe(CN)6 (3-/4-) redox probe, and their capacitive behavior in alkaline solutions. We correlate the electrochemical features with the presence of structural defects and oxygen functionalities on the graphene materials. In particular, the use of LiClO4 during the electrochemical exfoliation of graphite allowed the formation of highly oxidized graphene with a C/O ratio close to 4.0 and represents a possible avenue for the mass production of graphene oxide as valid alternative to the current laborious and dangerous chemical procedures, which also have limited scalability. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Solid oxide materials research accelerated electrochemical testing

    SciTech Connect

    Windisch, C.; Arey, B.

    1995-08-01

    The objectives of this work were to develop methods for accelerated testing of cathode materials for solid oxide fuel cells under selected operating conditions. The methods would be used to evaluate the performance of LSM cathode material.

  11. Improved Electrochemical Detection of Zinc Ions Using Electrode Modified with Electrochemically Reduced Graphene Oxide

    PubMed Central

    Kudr, Jiri; Richtera, Lukas; Nejdl, Lukas; Xhaxhiu, Kledi; Vitek, Petr; Rutkay-Nedecky, Branislav; Hynek, David; Kopel, Pavel; Adam, Vojtech; Kizek, Rene

    2016-01-01

    Increasing urbanization and industrialization lead to the release of metals into the biosphere, which has become a serious issue for public health. In this paper, the direct electrochemical reduction of zinc ions is studied using electrochemically reduced graphene oxide (ERGO) modified glassy carbon electrode (GCE). The graphene oxide (GO) was fabricated using modified Hummers method and was electrochemically reduced on the surface of GCE by performing cyclic voltammograms from 0 to −1.5 V. The modification was optimized and properties of electrodes were determined using electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The determination of Zn(II) was performed using differential pulse voltammetry technique, platinum wire as a counter electrode, and Ag/AgCl/3 M KCl reference electrode. Compared to the bare GCE the modified GCE/ERGO shows three times better electrocatalytic activity towards zinc ions, with an increase of reduction current along with a negative shift of reduction potential. Using GCE/ERGO detection limit 5 ng·mL−1 was obtained. PMID:28787832

  12. Co(III) as mediator in phenol destruction using electrochemical oxidation

    NASA Astrophysics Data System (ADS)

    Herlina, Herlina; Derlini, Derlini; Muhammad, Razali

    2017-03-01

    Mediated electrochemical oxidation is one of the method for oxidation of organic compound by using a mediator. This method has been developed because have several advantages which low cost and efficient, the exhaust gas does not contain toxic materials and hazardous waste and the process take place at a relatively low temperature. Electrochemical oxidation of organic compounds using metal ion mediator is one alternative method that is appropriate for the treatment of organic waste. Co(III) is a strong oxidizing agent used as a mediator has been prepared in Pt electrodes. The concentration of Co(III) formed during oxidation determined by potentiometric titration where Co(III) aliquot was added into Fe(II) excess solution and the remaining Fe(II) which did not react has been titrated with Ce(IV). In optimum condition, Co(III) was then used to oxidize the organic compound into carbon dioxide. The parameters has been studied are the standard oxidation potential of mediator, acid concentration and temperature. The results obtained at potential of 6 Volt, with nitric acid 4 M and temperature of 25°C give result 23.86% where Co (II) is converted to Co(III) within 2 hours. The addition of silver nitrate can increase the concentration of Co(III). At the optimum conditions, the mediator ion Co(III) can destructed to 66.44% of phenol compound oxidized into carbon dioxide.

  13. Electrochemical phase diagrams for Ti oxides from density functional calculations

    NASA Astrophysics Data System (ADS)

    Huang, Liang-Feng; Rondinelli, James M.

    2015-12-01

    Developing an accurate simulation method for the electrochemical stability of solids, as well as understanding the physics related with its accuracy, is critically important for improving the performance of compounds and predicting the stability of new materials in aqueous environments. Herein we propose a workflow for the accurate calculation of first-principles electrochemical phase (Pourbaix) diagrams. With this scheme, we study the electrochemical stabilities of Ti and Ti oxides using density-functional theory. First, we find the accuracy of an exchange-correlation functional in predicting formation energies and electrochemical stabilities is closely related with the electronic exchange interaction therein. Second, the metaGGA and hybrid functionals with a more precise description of the electronic exchange interaction lead to a systematic improvement in the accuracy of the Pourbaix diagrams. Furthermore, we show that accurate Ti Pourbaix diagrams also require that thermal effects are included through vibrational contributions to the free energy. We then use these diagrams to explain various experimental electrochemical phenomena for the Ti-O system, and show that if experimental formation energies for Ti oxides, which contain contributions from defects owing to their generation at high (combustion) temperatures, are directly used to predict room temperature Pourbaix diagrams then significant inaccuracies result. In contrast, the formation energies from accurate first-principles calculations, e.g., using metaGGA and hybrid functionals, are found to be more reliable. Finally, to facilitate the future application of our accurate electrochemical phase equilibria diagrams, the variation of the Ti Pourbaix diagrams with aqueous ion concentration is also provided.

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

    PubMed

    Oh, Misoon; Kim, Seok

    2012-01-01

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

  15. Electrochemical deposition of conducting ruthenium oxide films from solution

    SciTech Connect

    Anderson, D.P.; Warren, L.F.

    1984-02-01

    In the last decade, ruthenium oxide, RuO /sub x/ (x less than or equal to 2), has been used extensively as the active anode electrocatalyst constituent for Cl/sub 2/ and O/sub 2/ evolution reactions, in chlorate production, and in metal electrowinning from mixed chloride-sulfate solutions. More recently, this material has been incorporated in several light-induced water electrolysis schemes and apparently possesses the ability to inhibit CdS photocorrosion by acting as a hole scavenger. The numerous applications for this catalyst material certainly warrant further studies of its electrochemical properties on a variety of substrates, e.g., semiconductors. The lack of a simple technique for controlled deposition of ruthenium oxide onto conducting substrates prompted us to investigate an electrochemical approach to this problem. We describe here a new way to electrochemically deposit conducting films of hydrated ruthenium oxide from an aqueous solution of the benzeneruthenium (II)aqua complex. The films slowly dissolve in aqueous electrolytes upon potential cycling, yet appear to be catalytic with regards to water oxidation.

  16. Electrochemical properties of inorganic nanoporous oxide coated electrodes

    NASA Astrophysics Data System (ADS)

    Leonard, Kevin C.

    The ability to produce clean water and produce and store clean energy is essential to society. Hence, technologies that facilitate clean energy and clean water are of great importance. This study focused on utilizing nanoporous insulating oxide materials to alter the chemistry at the electrode/electrolyte interface to improve the performance of a number of clean energy and clean water technologies. Here we have shown that applying a thin-film of SiO2 nanoparticles to an electrochemical capacitor electrode can increase the energy storage capacity by up to 50% at high power ratings. We have developed a geometric model to describe the coating of the porous electrode to explain the increased performance at high power ratings. We have also shown that the coated electrochemical capacitor exhibits a higher capacitance when normalized to BET surface area, suggesting that the coated surface is behaving fundamentally differently than the uncoated surface. We attribute the increase in capacitance to the inherent surface potential of the oxide coating and have shown that if we alter the surface potential of the oxide, we can in turn alter the electrochemical capacitance. In addition, we have determined that when used in capacitive deionization systems, these coatings can increase ion removal and accelerate regeneration, allowing for higher efficiency and less waste water. We have demonstrated that a nanoporous oxide coating can increase the gas production rate and lower the overpotential of the hydrogen evolution reaction via water electrolysis on both stainless steel and carbon electrodes. In addition, this work presents data on utilizing nanoporous oxide coatings on Li-Ion battery cathodes to improve high temperature capacity fade. We also introduce a novel thin-film battery/electrochemical capacitor hybrid device, which can improve the performance of simple thin-film batteries.

  17. Direct electrochemical reduction of metal-oxides

    DOEpatents

    Redey, Laszlo I.; Gourishankar, Karthick

    2003-01-01

    A method of controlling the direct electrolytic reduction of a metal oxide or mixtures of metal oxides to the corresponding metal or metals. A non-consumable anode and a cathode and a salt electrolyte with a first reference electrode near the non-consumable anode and a second reference electrode near the cathode are used. Oxygen gas is produced and removed from the cell. The anode potential is compared to the first reference electrode to prevent anode dissolution and gas evolution other than oxygen, and the cathode potential is compared to the second reference electrode to prevent production of reductant metal from ions in the electrolyte.

  18. Electrochemical degradation of 4-chlorophenol at nickel-antimony doped tin oxide electrode.

    PubMed

    Wang, Y H; Chan, K Y; Li, X Y; So, S K

    2006-11-01

    The effectiveness of a novel nickel-antimony doped tin oxide electrode for electrochemical degradation of organic pollutants was investigated using 4-chlorophenol (4-CP) as a model toxic organic. The experimental results demonstrate that the optimal Ni content was at Ni:Sn=1:500 in atomic ratio in the precursor coating solution, whereas the Sb:Sn ratio was set at 8:500. Using the electrode prepared with the optimal Ni doping ratio for 4-CP degradation, the charge-based efficiencies were up to 89 microg C(-1) for 4-CP destruction and 15 microg C(-1) for TOC removal, which were considerably higher than the efficiencies observed for other electrodes. It is suggested that the enhancement of the electrode for electrochemical oxidation of organics could be attributed to the production of hydroxyl radicals in anodic water electrolysis.

  19. Electrochemical deposition of zinc oxide nanorods for hybrid solar cells

    NASA Astrophysics Data System (ADS)

    Torres Damasco Ty, Jennifer; Yanagi, Hisao

    2015-04-01

    Zinc oxide (ZnO) nanorod arrays for inorganic/organic hybrid solar cells were electrochemically deposited on indium tin oxide (ITO) substrates with a rotating disk electrode setup. The addition of a ZnO seed layer on the ITO prior to electrochemical deposition improved the morphology of the nanorods, resulting in nanorods with smaller and homogenous diameters as well as a higher degree of vertical orientation on to the substrate. The ZnO films deposited on the seeded ITO substrates had higher optical transmittance and lower concentration of defects. Chronoamperometric transient curves show that nucleation and coalescence occurred later for bare ITO substrates, indicating lower densities of initial nuclei, resulting in the growth of nanorods with larger diameters. The solar cell characteristics of the devices fabricated from the seeded ITO substrates were better. The seed layer also acts as a hole-blocking layer, preventing the direct contact between the hole-transporting polymer material and the ITO.

  20. Nitrogen-doped reduced graphene oxide electrodes for electrochemical supercapacitors.

    PubMed

    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.

  1. Electrochemical Oxidation of Synthetic Dyes in Simulated Wastewaters

    NASA Astrophysics Data System (ADS)

    Gallios, G.; Violintzis, X.; Voinovskii, I.; Voulgaropoulos, A.

    An electrochemical oxidation method for the degradation of synthetic reactive azodyes found in textile wastewaters is discussed. Four commercial synthetic dyes (black, blue, red and yellow) commonly used in dying operations were studied in single, binary and ternary mixtures. Low (100 mg/L) and high (500, 1,000 and 2,000 mg/L) initial dye concentrations were studied. The effect of various sodium chloride concentrations (as supporting electrolyte) on the effectiveness of electrochemical oxidation was examined. The effect of current intensity (1.5, 2.5 and 3.0 A) and pH (vales 3, 5, 7 and 10) was studied as well. The kinetics of the electrochemical oxidation for each dye were studied and compared. The conditions for effective dye degradation even from 2,000 mg/L initial concentration were established. The method was proved very effective even with binary and ternary mixtures of basic synthetic dyes. The Chemical Oxygen Demand (COD) and the Total Organic Carbon (TOC) were reduced by 60% and 25% respectively, meaning that the treated solutions were friendlier to the environment.

  2. Preparation and characterization of copper-doped cobalt oxide electrodes.

    PubMed

    Rosa-Toro, A La; Berenguer, R; Quijada, C; Montilla, F; Morallón, E; Vazquez, J L

    2006-11-30

    Cobalt oxide (Co3O4) and copper-doped cobalt oxide (CuxCo(3-x)O4) films have been prepared onto titanium support by the thermal decomposition method. The electrodes have been characterized by different techniques such as cyclic voltammetry, scanning electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy (XPS). The effect on the electrochemical and crystallographic properties and surface morphology of the amount of copper in the oxide layer has been analyzed. The XPS spectra correspond to a characteristic monophasic Cu-Co spinel oxides when x is below 1. However, when the copper content exceeds that for the stoichiometric CuCo2O4 spinel, a new CuO phase segregates at the surface. The analysis of the surface cation distribution indicates that Cu(II) has preference for octahedral sites.

  3. Electrochemical preparation and characterization of polypyrrole/stainless steel electrodes decorated with gold nanoparticles.

    PubMed

    Gutiérrez Pineda, Eduart; Alcaide, Francisco; Rodríguez Presa, María J; Bolzán, Agustín E; Gervasi, Claudio A

    2015-02-04

    The electrosynthesis and characterization of polypyrrole(PPy)/stainless steel electrodes decorated with gold nanoparticles and the performance of the composite electrode for sensing applications is described. PPy films were grown in potassium perchlorate and sodium salicylate solutions under comparable electropolymerization conditions. Polymer films prepared in the presence of perchlorate ions exhibited worm-like structures, whereas columnar structures were obtained in salicylate-containing solutions. Voltammetric response of PPy films prepared in salicylate solutions was more reversible. PPy films were decorated with gold nanoparticles obtained by a double step potentiostatic electrodeposition routine that allowed fine control of deposit characteristics. Analysis of deposits was performed by means of SEM and confocal Raman spectroscopy. The electrocatalytic activity of the Au/PPy electrodes was assessed for the electro-oxidation of hydrazine and hydroxylamine. Results showed a successful optimization of the route of synthesis that rendered nanocomposite electrode materials with promising applications in electrochemical sensing.

  4. Observable Electrochemical Oxidation of Carbon Promoted by Platinum Nanoparticles.

    PubMed

    Kou, Zongkui; Cheng, Kun; Wu, Hui; Sun, Ronghui; Guo, Beibei; Mu, Shichun

    2016-02-17

    The radical degradation of Pt-based catalysts toward oxygen reduction reaction (ORR), predominantly caused by the oxidation of carbon supports, heavily blocks the commercialization of polymer electrolyte membrane fuel cells (PEMFCs). As reported, the electrochemical oxidation of carbon could be accelerated by Pt catalysts; however, hitherto no direct evidence is present for the promotion of Pt catalysts. Herein, a unique ultrathin carbon layer (approximately 2.9 nm in thickness) covered Pt catalyst (Pt/C-GC) is designed and synthesized by a chemical vapor deposition (CVD) method. This magnifies the catalysis effect of Pt to carbon oxidation due to the greatly increased contact sites between the metal-support, making it easy to investigate the carbon oxidation process by observing the thinning of the carbon layer on Pt nanoparticles from TEM observations. Undoubtedly, this finding can better guide the structural design of the durable metal catalysts for PEMFCs and other applications.

  5. Electrochemical process for the preparation of nitrogen fertilizers

    DOEpatents

    Jiang, Junhua; Aulich, Ted R; Ignatchenko, Alexey V

    2015-04-14

    Methods and apparatus for the preparation of nitrogen fertilizers including ammonium nitrate, urea, urea-ammonium nitrate, and/or ammonia are disclosed. Embodiments include (1) ammonium nitrate produced via the reduction of a nitrogen source at the cathode and the oxidation of a nitrogen source at the anode; (2) urea or its isomers produced via the simultaneous cathodic reduction of a carbon source and a nitrogen source: (3) ammonia produced via the reduction of nitrogen source at the cathode and the oxidation of a hydrogen source or a hydrogen equivalent such as carbon monoxide or a mixture of carbon monoxide and hydrogen at the anode; and (4) urea-ammonium nitrate produced via the simultaneous cathodic reduction of a carbon source and a nitrogen source, and anodic oxidation of a nitrogen source.

  6. Electrochemical process for the preparation of nitrogen fertilizers

    DOEpatents

    Aulich, Ted R.; Olson, Edwin S.; Jiang, Junhua

    2013-03-19

    The present invention provides methods and apparatus for the preparation of nitrogen fertilizers including ammonium nitrate, urea, urea-ammonium nitrate, and/or ammonia utilizing a source of carbon, a source of nitrogen, and/or a source of hydrogen. Implementing an electrolyte serving as ionic charge carrier, (1) ammonium nitrate is produced via the reduction of a nitrogen source at the cathode and the oxidation of a nitrogen source at the anode; (2) urea or its isomers are produced via the simultaneous cathodic reduction of a carbon source and a nitrogen source; (3) ammonia is produced via the reduction of nitrogen source at the cathode and the oxidation of a hydrogen source at the anode; and (4) urea-ammonium nitrate is produced via the simultaneous cathodic reduction of a carbon source and a nitrogen source, and anodic oxidation of a nitrogen source. The electrolyte can be solid.

  7. Solar-powered electrochemical oxidation of organic compounds coupled with the cathodic production of molecular hydrogen.

    PubMed

    Park, Hyunwoong; Vecitis, Chad D; Hoffmann, Michael R

    2008-08-21

    A Bi-doped TiO2 anode, which is prepared from a mixed metal oxide coating deposited on Ti metal, is shown to be efficient for conventional water splitting. In this hybrid photovoltaic-electrochemical system, a photovoltaic (PV) cell is used to convert solar light to electricity, which is then used to oxidize a series of phenolic compounds at the semiconductor anode to carbon dioxide with the simultaneous production of molecular hydrogen from water/proton reduction at the stainless steel cathode. Degradation of phenol in the presence of a background NaCl electrolyte produces chlorinated phenols as reaction intermediates, which are subsequently oxidized completely to carbon dioxide and low-molecular weight carboxylic acids. The anodic current efficiency for the complete oxidation of phenolic compounds ranges from 3% to 17%, while the cathodic current efficiency and the energy efficiency for hydrogen gas generation range from 68% to 95% and 30% to 70%, respectively.

  8. Electrochemical preparation of the bis(ruthenocenium) dication.

    PubMed

    Trupia, Sabrina; Nafady, Ayman; Geiger, William E

    2003-09-08

    The electrochemical oxidation of ruthenocene (1) in CH(2)Cl(2)/[NBu(4)]A, where A = [B(C(6)F(5))(4)](-) or [B(C(6)H(3)(CF(3))(2))(4)](-), gives the dimeric dication [(RuCp(2))(2)](2+), 2(2+), in equilibrium with the 17-electron ruthenocenium ion 1(+). At room temperature the rapid equilibrium accounts for the quasi-Nernstian cyclic voltammetry (CV) behavior (E(1/2) = 0.41 V vs FeCp(2), A = [B(C(6)F(5))(4)](-)). Direct electrochemical evidence for 2(2+) is seen by CV and by bulk electrolysis at 243 K. The bis(ruthenocenium) dication undergoes a highly irreversible two-electron cathodic reaction at E(pc) ca. 0 V. Anodic electrolysis of 1 at 243 K using [B(C(6)H(3)(CF(3))(2))(4)](-) as the supporting electrolyte, followed by cathodic electrolysis of 2(2+), regenerates half of the original 1. Precipitation of 2(2+) occurs when the supporting electrolyte is [B(C(6)F(5))(4)](-), allowing facile isolation of [(RuCp(2))(2)][B(C(6)F(5))(4)](2). A second, unidentified, anodic product also reduces to give back ruthenocene. Digital simulations of the CV curves of 1 at 243 K give a dimerization equilibrium constant of 9 x 10(4) M(-1) for K(eq) = [(RuCp(2))(2)(2+)]/2 [RuCp(2)](+) in CH(2)Cl(2)/0.1 M [NBu(4)][B(C(6)F(5))(4)].

  9. Preparation and characterization of graphite fluorometallate salts and graphite fluorides by chemical and electrochemical methods

    SciTech Connect

    Lerner, M.M.

    1988-09-01

    Graphite intercalation compounds of main-group metal fluorides are prepared utilizing Cl/sub 2/ as an oxidizing agent. The action of Cl/sub 2/ with GeF/sub 4/ and Cl/sub 2//HF with either PF/sub 5/ or BF/sub 3/ on graphite produces fluorometallate salts. The relationship between the calculated enthalpy change for the reduction half-reaction and degree of intercalation is discussed. The electrochemical oxidation of graphite in 49% aqueous HF generates, at the oxidation limit, a 2nd stage graphite fluoride with a charge on carbon of C/sub 10/minus/14//sup /plus//. The fully-oxidized product is a 2nd stage analog of the planar-sheet graphite fluorides produced by the chemical or electrochemical fluorination of graphite in liquid anhydrous hydrogen fluoride (AHF). The fluorometallate salts prepared by electrochemical oxidation of graphite in an AHF/alkali metal fluorometallate salt (M = As, P, B, Sn) electrolyte are examined. The chemical fluorination of 2nd- and 3rd-stage C/sub x/AsF/sub 6/ salts with AHF/F/sub 2/ at ambient temperature produces a planar-sheet graphite fluoride phase with a C/F ratio as low as 1.3 along with a C/sub x/AsF/sub 6/ phase. The reaction of graphite with AHF/SnF/sub 4//F/sub 2/ results in the rapid disappearance of SnF/sub 4/, F/sub 2/ uptake, and color change of the solid from grey to blue-black. Graphite reacts with AHF/K/sub 2/MnF/sub 6/ in a stoichiometric ratio of at least 1 Mn for 6 C to produce MnF/sub 3/ and a C/sub x/F phase. The reaction of excess PF/sub 5/ with a well-evacuated C/sub x/BF/sub 4/ /center dot/ deltaBF/sub 3/ salt yields partial displacement of BF/sub 3/. When PF/sub 5/ /plus/ HF are employed, no BF/sub 3/ is displaced from the fluoroborate salt. 21 refs., 15 figs., 18 tabs.

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

    PubMed

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

    2017-06-21

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

  11. Oxidation of enrofloxacin with conductive-diamond electrochemical oxidation, ozonation and Fenton oxidation: a comparison.

    PubMed

    Guinea, Elena; Brillas, Enric; Centellas, Francesc; Cañizares, Pablo; Rodrigo, Manuel A; Sáez, Cristina

    2009-05-01

    The treatment of enrofloxacin synthetic wastewaters using conductive-diamond electrochemical oxidation (CDEO), ozonation and Fenton oxidation has been studied. Results show that the three technologies can reduce the organic content of enrofloxacin synthetic wastewaters but with different performances. CDEO was the most efficient technology in terms of mineralization but not on COD removal, which was more efficiently achieved by ozonation. This indicates that ozonation is efficient in the breakage of the complex molecules but not on the removal of final carboxylic acids. The high initial efficiency in terms of oxidant-use obtained by Fenton oxidation evidences that it is very efficient in the removal of the enrofloxacin, although it rapidly leads to the formation of refractory compounds to the treatment. This indicates the significance of other oxidation mechanisms (e.g. coagulation) that enhance the results obtained by the expected hydroxyl-mediated oxidation. Ammonium ions were the primary product species in CDEO and nitrate ions in ozonation, whereas Fenton effluents contained similar amounts of both nitrogen ionic species.

  12. Method for preparing hollow metal oxide microsphere

    DOEpatents

    Schmitt, C.R.

    1974-02-12

    Hollow refractory metal oxide microspheres are prepared by impregnating resinous microspheres with a metallic compound, drying the impregnated microspheres, heating the microspheres slowly to carbonize the resin, and igniting the microspheres to remove the carbon and to produce the metal oxide. Zirconium oxide is given as an example. (Official Gazette)

  13. [Effect of pH for the electrochemical oxidation products and oxidation pathways of ammonia].

    PubMed

    Chen, Jin-luan; Shi, Han-chang; Xu, Li-li

    2008-08-01

    The electrochemical oxidation of ammonia in wastewater was investigated in a flow electrochemical cell. The effect of pH on ammonia removal efficiency, oxidation products and oxidation pathways was elucidated. The experimental results indicated that, the higher production efficiency of free chlorine and hydroxyl radical can be obtained under the moderate alkaline condition, and the electrochemical oxidation rate of ammonia was higher in this condition. In existence of chloride ions, chloramines produced during the electrolysis of ammonia. The constituent of chloramines related with the pH of reaction system. When pH was higher than 9, monochloramine was dominant; When pH was equal to 7, monochloramine and dichloramine existed at the same time and the concentration of the two chloramines was an approximation of the same; When pH was smaller than 5, most of the production was dichloramine. The production of nitrogen trichloride can be avoided when pH was higher than 5. Under the current density of 20 mA/cm2, the concentration of hydroxyl radical produced by electrolysis was smaller than 5 x 10(-15) mol/L. The indirect oxidation was the dominant reaction in the two pathways of electrochemical oxidation of ammonia.

  14. Preparation and electrochemistry of one-dimensional nanostructured MnO 2/PPy composite for electrochemical capacitor

    NASA Astrophysics Data System (ADS)

    Li, Juan; Cui, Li; Zhang, Xiaogang

    2010-04-01

    One-dimensional nanostructured manganese dioxide/polypyrrole (MnO 2/PPy) composite was prepared by in situ chemical oxidation polymerization of pyrrole in the host of inorganic matrix of MnO 2, using complex of methyl orange (MO)/FeCl 3 as a reactive self-degraded soft-template. The morphology and structure of the composite were characterized by infrared spectroscopy (IR) X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results show that the MnO 2/PPy composite consists of α-MnO 2 and PPy with nanotube-like structure. Electrochemical properties of the composite demonstrated the material showed good electrochemical reversibility after 500 charge-discharge cycles in the potential range of -0.4 to 0.6 V, the tube-like nanocomposite has the potential application in electrochemical capacitor.

  15. Electrochemical oxidation by square-wave potential pulses in the imitation of oxidative drug metabolism.

    PubMed

    Nouri-Nigjeh, Eslam; Permentier, Hjalmar P; Bischoff, Rainer; Bruins, Andries P

    2011-07-15

    Electrochemistry combined with mass spectrometry (EC-MS) is an emerging analytical technique in the imitation of oxidative drug metabolism at the early stages of new drug development. Here, we present the benefits of electrochemical oxidation by square-wave potential pulses for the oxidation of lidocaine, a test drug compound, on a platinum electrode. Lidocaine was oxidized at constant potential and by square-wave potential pulses with different cycle times, and the reaction products were analyzed by liquid chromatography-mass spectrometry [LC-MS(/MS)]. Application of constant potentials of up to +5.0 V resulted in relatively low yields of N-dealkylation and 4-hydroxylation products, while oxidation by square-wave potential pulses generated up to 50 times more of the 4-hydroxylation product at cycle times between 0.2 and 12 s (estimated yield of 10%). The highest yield of the N-dealkylation product was obtained at cycle times shorter than 0.2 s. Tuning of the cycle time is thus an important parameter to modulate the selectivity of electrochemical oxidation reactions. The N-oxidation product was only obtained by electrochemical oxidation under air atmosphere due to reaction with electrogenerated hydrogen peroxide. Square-wave potential pulses may also be applicable to modulate the selectivity of electrochemical reactions with other drug compounds in order to generate oxidation products with greater selectivity and higher yield based on the optimization of cycle times and potentials. This considerably widens the scope of direct electrochemistry-based oxidation reactions for the imitation of in vivo oxidative drug metabolism.

  16. Fabrication of solid oxide fuel cell by electrochemical vapor deposition

    DOEpatents

    Brian, Riley; Szreders, Bernard E.

    1989-01-01

    In a high temperature solid oxide fuel cell (SOFC), the deposition of an impervious high density thin layer of electrically conductive interconnector material, such as magnesium doped lanthanum chromite, and of an electrolyte material, such as yttria stabilized zirconia, onto a porous support/air electrode substrate surface is carried out at high temperatures (approximately 1100.degree.-1300.degree. C.) by a process of electrochemical vapor deposition. In this process, the mixed chlorides of the specific metals involved react in the gaseous state with water vapor resulting in the deposit of an impervious thin oxide layer on the support tube/air electrode substrate of between 20-50 microns in thickness. An internal heater, such as a heat pipe, is placed within the support tube/air electrode substrate and induces a uniform temperature profile therein so as to afford precise and uniform oxide deposition kinetics in an arrangement which is particularly adapted for large scale, commercial fabrication of SOFCs.

  17. Fabrication of solid oxide fuel cell by electrochemical vapor deposition

    DOEpatents

    Riley, B.; Szreders, B.E.

    1988-04-26

    In a high temperature solid oxide fuel cell (SOFC), the deposition of an impervious high density thin layer of electrically conductive interconnector material, such as magnesium doped lanthanum chromite, and of an electrolyte material, such as yttria stabilized zirconia, onto a porous support/air electrode substrate surface is carried out at high temperatures (/approximately/1100/degree/ /minus/ 1300/degree/C) by a process of electrochemical vapor deposition. In this process, the mixed chlorides of the specific metals involved react in the gaseous state with water vapor resulting in the deposit of an impervious thin oxide layer on the support tube/air electrode substrate of between 20--50 microns in thickness. An internal heater, such as a heat pipe, is placed within the support tube/air electrode substrate and induces a uniform temperature profile therein so as to afford precise and uniform oxide deposition kinetics in an arrangement which is particularly adapted for large scale, commercial fabrication of SOFCs.

  18. Chitosan-iron oxide nanocomposite based electrochemical aptasensor for determination of malathion.

    PubMed

    Prabhakar, Nirmal; Thakur, Himkusha; Bharti, Anu; Kaur, Navpreet

    2016-10-05

    An electrochemical aptasensor based on chitosan-iron oxide nanocomposite (CHIT-IO) film deposited on fluorine tin Oxide (FTO) was developed for the detection of malathion. Iron oxide nanoparticles were prepared by co-precipitation method and characterized by Transmission electron microscopy and UV-Visible spectroscopy. The biotinylated DNA aptamer sequence specific to the malathion was immobilized onto the iron oxide doped-chitosan/FTO electrode by using streptavidin as linking molecule. Various characterization studies like Field Emission-Scanning Electron Microscopy (FE-SEM), Fourier Transform Infrared Spectroscopy (FT-IR), and Electrochemical studies were performed to attest the successful fabrication of bioelectrodes. Experimental parameters like aptamer concentration, response time, stability of electrode and reusability studies were optimized. Aptamer immobilized chitosan-iron oxide nanocomposite (APT/SA/CHIT-IO/FTO) bioelectrodes exhibited LOD of about 0.001 ng/mL within 15 min and spike-in studies revealed about 80-92% recovery of malathion from the lettuce leaves and soil sample. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Scalable and sustainable electrochemical allylic C-H oxidation.

    PubMed

    Horn, Evan J; Rosen, Brandon R; Chen, Yong; Tang, Jiaze; Chen, Ke; Eastgate, Martin D; Baran, Phil S

    2016-05-05

    New methods and strategies for the direct functionalization of C-H bonds are beginning to reshape the field of retrosynthetic analysis, affecting the synthesis of natural products, medicines and materials. The oxidation of allylic systems has played a prominent role in this context as possibly the most widely applied C-H functionalization, owing to the utility of enones and allylic alcohols as versatile intermediates, and their prevalence in natural and unnatural materials. Allylic oxidations have featured in hundreds of syntheses, including some natural product syntheses regarded as "classics". Despite many attempts to improve the efficiency and practicality of this transformation, the majority of conditions still use highly toxic reagents (based around toxic elements such as chromium or selenium) or expensive catalysts (such as palladium or rhodium). These requirements are problematic in industrial settings; currently, no scalable and sustainable solution to allylic oxidation exists. This oxidation strategy is therefore rarely used for large-scale synthetic applications, limiting the adoption of this retrosynthetic strategy by industrial scientists. Here we describe an electrochemical C-H oxidation strategy that exhibits broad substrate scope, operational simplicity and high chemoselectivity. It uses inexpensive and readily available materials, and represents a scalable allylic C-H oxidation (demonstrated on 100 grams), enabling the adoption of this C-H oxidation strategy in large-scale industrial settings without substantial environmental impact.

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

    PubMed

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

    2017-05-01

    A novel lobetyolin electrochemical sensor based on a magnetic functionalized reduced graphene oxide/Nafion nanohybrid film has been introduced in this work. The magnetic functionalized reduced graphene oxide was characterized by fourier transform infrared spectroscopy, atomic force microscope, X-ray diffraction, transmission electron microscopy and thermogravimetric analysis. The scanning electron microscopy characterized the morphology and microstructure of the prepared sensors, and the electrochemical effective surface areas of the prepared sensors were also calculated by chronocoulometry method. The electrochemical behavior of lobetyolin on the magnetic functionalized reduced graphene oxide/Nafion nanohybrid modified glassy carbon electrode was investigated by cyclic voltammetry and differential pulse voltammetry in a phosphate buffer solution of pH6.0. The electron-transfer coefficient (α), electron transfer number (n), and electrode reaction rate constant (Κs) were calculated as 0.78, 0.73, and 4.63s(-1), respectively. Under the optimized conditions, the sensor based on magnetic functionalized reduced graphene oxide/Nafion showed a linear voltammetric response to the lobetyolin concentration at 1.0×10(-7) to 1.0×10(-4)mol/L with detection limit (S/N=3)of 4.3×10(-8)mol/L. The proposed sensor also displayed acceptable reproducibility, long-term stability, and high selectivity, and performs well for analysis of lobetyolin in real samples. The voltammetric sensor was successfully applied to detect lobetyolin in Codonopsis pilosula with recovery values in the range of 96.12%-102.66%.

  1. FTIR Spectra and Normal-Mode Analysis of a Tetranuclear Manganese Adamantane-like Complex in Two Electrochemically Prepared Oxidation States: Relevance to the Oxygen-Evolving Complex of Photosystem II

    PubMed Central

    Visser, Hendrik; Dubé, Christopher E.; Armstrong, William H.; Sauer, Kenneth; Yachandra, Vittal K.

    2014-01-01

    The IR spectra and normal-mode analysis of the adamantane-like compound [Mn4O6(bpea)4]n+ (bpea = N,N-bis(2-pyridylmethyl)ethylamine) in two oxidation states, MnIV4 and MnIIIMnIV3, that are relevant to the oxygen-evolving complex of photosystem II are presented. Mn–O vibrational modes are identified with isotopic exchange, 16O→18O, of the mono-μ-oxo bridging atoms in the complex. IR spectra of the MnIIIMnIV3 species are obtained by electrochemical reduction of the MnIV4 species using a spectroelectrochemical cell, based on attenuated total reflection [Visser, H.; et al. Anal. Chem. 2001, 73, 4374–4378]. A novel method of subtraction is used to reduce background contributions from solvent and ligand modes, and the difference and double-difference spectra are used in identifying Mn–O bridging modes that are sensitive to oxidation state change. Two strong IR bands are observed for the MnIV4 species at 745 and 707 cm−1, and a weaker band is observed at 510 cm−1. Upon reduction, the MnIIIMnIV3 species exhibits two strong IR bands at 745 and 680 cm−1, and several weaker bands are observed in the 510–425 cm−1 range. A normal-mode analysis is performed to assign all the relevant bridging modes in the oxidized MnIV4 and reduced MnIIIMnIV3 species. The calculated force constants for the MnIV4 species are frIV = 3.15 mdyn/Å, frOr = 0.55 mdyn/Å, and frMnr = 0.20 mdyn/Å. The force constants for the MnIIIMnIV3 species are frIV = 3.10 mdyn/Å, frIII = 2.45 mdyn/Å, frOr = 0.40 mdyn/Å, and frMnr = 0.15 mdyn/Å. This study provides insights for the identification of Mn–O modes in the IR spectra of the photosynthetic oxygen-evolving complex during its catalytic cycle. PMID:12224948

  2. FTIR spectra and normal-mode analysis of a tetranuclear manganese adamantane-like complex in two electrochemically prepared oxidation states: relevance to the oxygen-evolving complex of photosystem II.

    PubMed

    Visser, Hendrik; Dubé, Christopher E; Armstrong, William H; Sauer, Kenneth; Yachandra, Vittal K

    2002-09-18

    The IR spectra and normal-mode analysis of the adamantane-like compound [Mn(4)O(6)(bpea)(4)](n+) (bpea = N,N-bis(2-pyridylmethyl)ethylamine) in two oxidation states, Mn(IV)(4) and Mn(III)Mn(IV)(3), that are relevant to the oxygen-evolving complex of photosystem II are presented. Mn-O vibrational modes are identified with isotopic exchange, (16)O-->(18)O, of the mono-micro-oxo bridging atoms in the complex. IR spectra of the Mn(III)Mn(IV)(3) species are obtained by electrochemical reduction of the Mn(IV)(4) species using a spectroelectrochemical cell, based on attenuated total reflection [Visser, H.; et al. Anal. Chem. 2001, 73, 4374-4378]. A novel method of subtraction is used to reduce background contributions from solvent and ligand modes, and the difference and double-difference spectra are used in identifying Mn-O bridging modes that are sensitive to oxidation state change. Two strong IR bands are observed for the Mn(IV)(4) species at 745 and 707 cm(-1), and a weaker band is observed at 510 cm(-1). Upon reduction, the Mn(III)Mn(IV)(3) species exhibits two strong IR bands at 745 and 680 cm(-1), and several weaker bands are observed in the 510-425 cm(-1) range. A normal-mode analysis is performed to assign all the relevant bridging modes in the oxidized Mn(IV)(4) and reduced Mn(III)Mn(IV)(3) species. The calculated force constants for the Mn(IV)(4) species are f(r)(IV)= 3.15 mdyn/A, f(rOr) = 0.55 mdyn/A, and f(rMnr) = 0.20 mdyn/A. The force constants for the Mn(III)Mn(IV)(3) species are f(r)(IV)= 3.10 mdyn/A, f(r)(III)= 2.45 mdyn/A, f(rOr) = 0.40 mdyn/A, and f(rMnr) = 0.15 mdyn/A. This study provides insights for the identification of Mn-O modes in the IR spectra of the photosynthetic oxygen-evolving complex during its catalytic cycle.

  3. FTIR spectra and normal-mode analysis of a tetranuclear Manganese adamantane-like complex in two electrochemically prepared oxidation states: Relevance to the oxygen-evolving complex of Photosystem II

    SciTech Connect

    Visser, Hendrik; Dube, Christopher E.; Armstrong, William H.; Sauer, Kenneth; Yachandra, Vittal K.

    2002-03-19

    The IR spectra and normal-mode analysis of the adamantane-like compound [Mn4O6(bpea)4]n+ in two oxidation states, MnIV4 and MnIIIMnIV3, that are relevant to the oxygen-evolving complex of photosystem II are presented. Mn-O vibrational modes are identified with isotopic exchange, 16O->18O, of the mono-(mu)-oxo bridging atoms in the complex. IR spectra of the MnIIIMnIV3 species are obtained by electrochemical reduction of the MnIV4 species using a spectroelectrochemical cell, based on attenuated total reflection [Visser et al. Anal Chem 2001, 73, 4374-4378]. A novel method of subtraction is used to reduce background contributions from solvent and ligand modes, and the difference and double-difference spectra are used in identifying Mn-O bridging modes that are sensitive to oxidation state change. Two strong IR bands are observed for the MnIV4 species at 745 and 707 cm-1 and a weaker band at 510 cm-1. Upon reduction, the MnIIIMnIV3 species exhibits two strong IR bands at 745 and 680 cm-1, and several weaker bands are observed in the 510 - 425 cm-1 range. A normal mode analysis is performed to assign all the relevant bridging modes in the oxidized MnIV4 and reduced MnIIIMnIV3 species. The calculated force constants for the MnIV4 species are = 3.15 mdynAngstrom, = 0.55 mdyn/Angstrom, and = 0.20 mdyn/Angstrom. The force constants for the MnIIIMnIV3 species are = 3.10 mdyn/Angstrom, = 2.45 mdyn/Angstrom, = 0.40, and = 0.15 mdyn/Angstrom. This study provides insights for the identification of Mn-O modes in the IR spectra of the photosynthetic oxygen-evolving complex during its catalytic cycle.

  4. Preparation, characterization, and electrochemical performances of graphene/Ni(OH)2 hybrid nanomaterials

    NASA Astrophysics Data System (ADS)

    Yang, Duanguang; Wang, Fan; Yan, Jing; Gao, Yong; Li, Huaming

    2013-06-01

    Graphene-based hybrid nanomaterials have recently been investigated and proposed as a promising platform for electronic, optoelectronic, and electrochemical devices because of their high-surface area, remarkable chemical stability, and electrical conductivity. In this study, we demonstrated a facile method for the preparation of graphene/Ni(OH)2 hybrid nanomaterials. First, polymer-functionalized graphene oxide (PGO) was prepared by Cu(I)-catalyzed click coupling of alkyne-functionalized graphene oxide with azide-terminated poly(vinylpyrrolidone). Subsequently, Ni(OH)2 nanoparticles were deposited onto graphene nanosheets using PGO as a template. Upon reduction with NaBH4, graphene/Ni(OH)2 hybrid nanostructures were constructed. The as-prepared graphene/Ni(OH)2 hybrid nanosheets were directly immobilized onto the surface of glassy carbon electrode for glucose determination. The as-fabricated nonenzymatic glucose sensor exhibited a wider linearity range from 0.3 to 750 μM with a detection limit of 30 nM ( S/ N = 3).

  5. Electrochemical Detection of Nitric Oxide in Plant Cell Suspensions.

    PubMed

    Griveau, Sophie; Besson-Bard, Angélique; Bedioui, Fethi; Wendehenne, David

    2016-01-01

    Nitric oxide is a hydrophobic radical acting as a physiological mediator in plants. Because of its unique properties, the detection of NO in plant tissues and cell suspensions remains a challenge. For this purpose, several techniques are used, each having certain advantages and limitations such as interferences with other species, questionable sensitivity, and/or selectivity or ex situ measurement. Here we describe a very attractive approach for tracking NO in plant cell suspensions using a NO-sensitive homemade platinum/iridium-based electrochemical microsensor. This method constitutes the absolute real-time proof of the production of free NO in physiological conditions.

  6. Corner heating in rectangular solid oxide electrochemical cell generators

    DOEpatents

    Reichner, Philip

    1989-01-01

    Disclosed is an improvement in a solid oxide electrochemical cell generator 1 having a rectangular design with four sides that meet at corners, and containing multiplicity of electrically connected fuel cells 11, where a fuel gas is passed over one side of said cells and an oxygen containing gas is passed into said cells, and said fuel is burned to form heat, electricity, and an exhaust gas. The improvement comprises passing the exhaust gases over the multiplicity of cells 11 in such a way that more of the heat in said exhaust gases flows at the corners of the generator, such as through channels 19.

  7. Microwave synthesis and electrochemical characterization of Mn/Ni mixed oxide for supercapacitor application

    SciTech Connect

    Prasankumar, T.; Jose, Sujin P.; Ilangovan, R.; Venkatesh, K. S.

    2015-06-24

    Nanostructured Mn/Ni mixed metal oxide was synthesized at ambient temperature by facile microwave irradiation technique. The crystal structure and surface morphology were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. X-ray diffraction analysis confirmed the formation of Mn/Ni mixed oxide in rhombohedral phase and the grain size calculated was found to be 87 nm. The irregular spherical morphology of the prepared sample was exhibited by the SEM images. The characteristic peaks of FTIR at about 630 cm{sup −1} and 749 cm{sup −1} were attributed to the Mn-O and Ni-O stretching vibrations respectively. The presence of both Mn and Ni in the prepared sample was validated by the EDS spectra which in turn confirmed the formation of mixed oxide. Cyclic voltammetry and galvanostatic chargedischarge measurements were employed to investigate the electrochemical performance of the mixed oxide. The cyclic voltammetry curves demonstrated good capacitive performance of the sample in the potential window −0.2V to 0.9V. The charge discharge study revealed the suitability of the prepared mixed oxide for the fabrication of supercapacitor electrode.

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

    ERIC Educational Resources Information Center

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

    2008-01-01

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

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

    ERIC Educational Resources Information Center

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

    2008-01-01

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

  10. Scalable and Sustainable Electrochemical Allylic C–H Oxidation

    PubMed Central

    Chen, Yong; Tang, Jiaze; Chen, Ke; Eastgate, Martin D.; Baran, Phil S.

    2016-01-01

    New methods and strategies for the direct functionalization of C–H bonds are beginning to reshape the fabric of retrosynthetic analysis, impacting the synthesis of natural products, medicines, and even materials1. The oxidation of allylic systems has played a prominent role in this context as possibly the most widely applied C–H functionalization due to the utility of enones and allylic alcohols as versatile intermediates, along with their prevalence in natural and unnatural materials2. Allylic oxidations have been featured in hundreds of syntheses, including some natural product syntheses regarded as “classics”3. Despite many attempts to improve the efficiency and practicality of this powerful transformation, the vast majority of conditions still employ highly toxic reagents (based around toxic elements such as chromium, selenium, etc.) or expensive catalysts (palladium, rhodium, etc.)2. These requirements are highly problematic in industrial settings; currently, no scalable and sustainable solution to allylic oxidation exists. As such, this oxidation strategy is rarely embraced for large-scale synthetic applications, limiting the adoption of this important retrosynthetic strategy by industrial scientists. In this manuscript, we describe an electrochemical solution to this problem that exhibits broad substrate scope, operational simplicity, and high chemoselectivity. This method employs inexpensive and readily available materials, representing the first example of a scalable allylic C–H oxidation (demonstrated on 100 grams), finally opening the door for the adoption of this C–H oxidation strategy in large-scale industrial settings without significant environmental impact. PMID:27096371

  11. Electrochemical degradation, kinetics & performance studies of solid oxide fuel cells

    NASA Astrophysics Data System (ADS)

    Das, Debanjan

    Linear and Non-linear electrochemical characterization techniques and equivalent circuit modelling were carried out on miniature and sub-commercial Solid Oxide Fuel Cell (SOFC) stacks as an in-situ diagnostic approach to evaluate and analyze their performance under the presence of simulated alternative fuel conditions. The main focus of the study was to track the change in cell behavior and response live, as the cell was generating power. Electrochemical Impedance Spectroscopy (EIS) was the most important linear AC technique used for the study. The distinct effects of inorganic components usually present in hydrocarbon fuel reformates on SOFC behavior have been determined, allowing identification of possible "fingerprint" impedance behavior corresponding to specific fuel conditions and reaction mechanisms. Critical electrochemical processes and degradation mechanisms which might affect cell performance were identified and quantified. Sulfur and siloxane cause the most prominent degradation and the associated electrochemical cell parameters such as Gerisher and Warburg elements are applied respectively for better understanding of the degradation processes. Electrochemical Frequency Modulation (EFM) was applied for kinetic studies in SOFCs for the very first time for estimating the exchange current density and transfer coefficients. EFM is a non-linear in-situ electrochemical technique conceptually different from EIS and is used extensively in corrosion work, but rarely used on fuel cells till now. EFM is based on exploring information obtained from non-linear higher harmonic contributions from potential perturbations of electrochemical systems, otherwise not obtained by EIS. The baseline fuel used was 3 % humidified hydrogen with a 5-cell SOFC sub-commercial planar stack to perform the analysis. Traditional methods such as EIS and Tafel analysis were carried out at similar operating conditions to verify and correlate with the EFM data and ensure the validity of the

  12. Effect of additive on electrochemical corrosion properties of plasma electrolytic oxidation coatings formed on CP Ti under different processing frequency

    NASA Astrophysics Data System (ADS)

    Babaei, Mahdi; Dehghanian, Changiz; Vanaki, Mojtaba

    2015-12-01

    The plasma electrolytic oxidation (PEO) coating containing zirconium oxide was fabricated on CP Ti at different processing frequencies viz., 100 Hz and 1000 Hz in a (Na2ZrO3, Na2SiO3)-additive containing NaH2PO4-based solution, and long-term electrochemical corrosion behavior of the coatings was studied using electrochemical impedance spectroscopy (EIS) in 3.5 wt.% NaCl solution. Electrochemical degradation behavior of two-layered coatings formed at different frequencies was turned out to be governed by concentration of electrolyte additive. With increasing additive concentration, the coating obtained at frequency of 1000 Hz exhibited enhanced corrosion resistance. However, corrosion resistance of the coating prepared at 100 Hz was found to decrease with increased additive, which was attributed to intensified microdischarges damaging the protective effect of inner layer. Nevertheless, the electrolyte additive was found to mitigate the long-term degradation of the coatings to a significant extent.

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

    NASA Astrophysics Data System (ADS)

    Zhang, Yan; Hao, Huilian; Wang, Linlin

    2016-12-01

    Electrochemically reduced graphene oxide (ERGO) is widely used to construct electrochemical sensors. Understanding the electron transfer behavior of ERGO is essential for its electrode material applications. In this paper, different morphologies of ERGO were prepared via two different methods. Compared to ERGO/GCEs prepared by electrochemical reduction of pre-deposited GO, more exposed edge planes of ERGO are observed on the surface of ERGO-GCE that was constructed by electrophoretic deposition of GO. The defect densities of ERGO were controlled by tuning the mass or concentration of GO. The electron transfer kinetics (k0) of GCE with different ERGOs was comparatively investigated. Owing to increased surface areas and decreased defect density, the k0 values of ERGO/GCE initially increase and then decrease with incrementing of GO mass. When the morphology and surface real areas of ERGO-GCE are the same, an increased defect density induces an accelerated electron transfer rate. k0 valuesof ERGO-GCEs are about 1 order of magnitude higher than those of ERGO/GCEs due to the difference in the amount of edge planes. This work demonstrates that both defect densities and edge planes of ERGO play crucial roles in electron transfer kinetics.

  14. Electrochemical DNA biosensors based on thin gold films sputtered on capacitive nanoporous niobium oxide.

    PubMed

    Rho, Sangchul; Jahng, Deokjin; Lim, Jae Hoon; Choi, Jinsub; Chang, Jeong Ho; Lee, Sang Cheon; Kim, Kyung Ja

    2008-01-18

    Electrochemical DNA biosensors based on a thin gold film sputtered on anodic porous niobium oxide (Au@Nb(2)O(5)) are studied in detail here. We found that the novel DNA biosensor based on Au@Nb(2)O(5) is superior to those based on the bulk gold electrode or niobium oxide electrode. For example, the novel method does not require any time-consuming cleaning step in order to obtain reproducible results. The adhesion of gold films on the substrate is very stable during electrochemical biosensing, when the thin gold films are deposited on anodically prepared nanoporous niobium oxide. In particular, the novel biosensor shows enhanced biosensing performance with a 2.4 times higher resolution and a three times higher sensitivity. The signal enhancement is in part attributed to capacitive interface between gold films and nanoporous niobium oxide, where charges are accumulated during the anodic and cathodic scanning, and is in part ascribed to the structural stability of DNA immobilized at the sputtered gold films. The method allows for the detection of single-base mismatch DNA as well as for the discrimination of mismatch positions.

  15. Graphenes prepared by Staudenmaier, Hofmann and Hummers methods with consequent thermal exfoliation exhibit very different electrochemical properties

    NASA Astrophysics Data System (ADS)

    Poh, Hwee Ling; Šaněk, Filip; Ambrosi, Adriano; Zhao, Guanjia; Sofer, Zdeněk; Pumera, Martin

    2012-05-01

    Large-scale fabrication of graphene is highly important for industrial and academic applications of this material. The most common large-scale preparation method is the oxidation of graphite to graphite oxide using concentrated acids in the presence of strong oxidants and consequent thermal exfoliation and reduction by thermal shock to produce reduced graphene. These oxidation methods typically use concentrated sulfuric acid (a) in combination with fuming nitric acid and KClO3 (Staudenmaier method), (b) in combination with concentrated nitric acid and KClO3 (Hofmann method) or (c) in the absence of nitric acid but in the presence of NaNO3 and KMnO4 (Hummers method). The evaluation of quality and applicability of the graphenes produced by these various methods is of high importance and is attempted side-by-side for the first time in this paper. Full-scale characterization of thermally reduced graphenes prepared by these standard methods was performed with techniques such as transmission and scanning electron microscopy, Raman spectroscopy and X-ray photoelectron spectroscopy. Their applicability for electrochemical devices was further evaluated by means of cyclic voltammetry techniques. We showed that while Staudenmaier and Hofmann methods (methods that do not use potassium permanganate as oxidant) generated thermally reduced graphenes with comparable electrochemical properties, the graphene prepared by the Hummers method which uses permanganate as oxidant showed higher heterogeneous electron transfer rates and lower overpotentials as compared to graphenes prepared by the Staudenmaier or Hofmann methods. This clearly shows that the methods of preparations have dramatic influences on the materials properties and, thus, such findings are of eminent importance for practical applications as well as for academic research.

  16. Graphenes prepared by Staudenmaier, Hofmann and Hummers methods with consequent thermal exfoliation exhibit very different electrochemical properties.

    PubMed

    Poh, Hwee Ling; Šaněk, Filip; Ambrosi, Adriano; Zhao, Guanjia; Sofer, Zdeněk; Pumera, Martin

    2012-06-07

    Large-scale fabrication of graphene is highly important for industrial and academic applications of this material. The most common large-scale preparation method is the oxidation of graphite to graphite oxide using concentrated acids in the presence of strong oxidants and consequent thermal exfoliation and reduction by thermal shock to produce reduced graphene. These oxidation methods typically use concentrated sulfuric acid (a) in combination with fuming nitric acid and KClO(3) (Staudenmaier method), (b) in combination with concentrated nitric acid and KClO(3) (Hofmann method) or (c) in the absence of nitric acid but in the presence of NaNO(3) and KMnO(4) (Hummers method). The evaluation of quality and applicability of the graphenes produced by these various methods is of high importance and is attempted side-by-side for the first time in this paper. Full-scale characterization of thermally reduced graphenes prepared by these standard methods was performed with techniques such as transmission and scanning electron microscopy, Raman spectroscopy and X-ray photoelectron spectroscopy. Their applicability for electrochemical devices was further evaluated by means of cyclic voltammetry techniques. We showed that while Staudenmaier and Hofmann methods (methods that do not use potassium permanganate as oxidant) generated thermally reduced graphenes with comparable electrochemical properties, the graphene prepared by the Hummers method which uses permanganate as oxidant showed higher heterogeneous electron transfer rates and lower overpotentials as compared to graphenes prepared by the Staudenmaier or Hofmann methods. This clearly shows that the methods of preparations have dramatic influences on the materials properties and, thus, such findings are of eminent importance for practical applications as well as for academic research.

  17. Electrochemical process for the preparation of nitrogen fertilizers

    DOEpatents

    Aulich, Ted R [Grand Forks, ND; Olson, Edwin S [Grand Forks, ND; Jiang, Junhua [Grand Forks, ND

    2012-04-10

    The present invention provides methods and apparatus for the preparation of nitrogen fertilizers including ammonium nitrate, urea, urea-ammonium nitrate, and/or ammonia, at low temperature and pressure, preferably at ambient temperature and pressure, utilizing a source of carbon, a source of nitrogen, and/or a source of hydrogen or hydrogen equivalent. Implementing an electrolyte serving as ionic charge carrier, (1) ammonium nitrate is produced via the reduction of a nitrogen source at the cathode and the oxidation of a nitrogen source at the anode; (2) urea or its isomers are produced via the simultaneous cathodic reduction of a carbon source and a nitrogen source; (3) ammonia is produced via the reduction of nitrogen source at the cathode and the oxidation of a hydrogen source or a hydrogen equivalent such as carbon monoxide or a mixture of carbon monoxide and hydrogen at the anode; and (4) urea-ammonium nitrate is produced via the simultaneous cathodic reduction of a carbon source and a nitrogen source, and anodic oxidation of a nitrogen source. The electrolyte can be aqueous, non-aqueous, or solid.

  18. Mediated Electrochemical Oxidation (MEO) based technology. Final report

    SciTech Connect

    1996-07-18

    The goal of this CRADA was the continued research and development by LLNL, and the commercialization by EOSystems, Inc., of the waste treatment technology known as Mediated Electrochemical Oxidation. MEO is a non-thermal electrochemical technology developed in part at LLNL for the destruction of organic waste streams; this technology has wide applications in the government, manufacturing, biomedical and industrial sectors. The system uses an electrochemical cell to generate highly oxidizing {open_quote}mediators{close_quote} in an acidic aqueous solution, which subsequently react with organic waste and convert it to carbon dioxide and water. The broad research responsibilities of LLNL in this CRADA were the investigation of numerous cell electrode materials and materials of construction, the evaluation of the process chemistry, and the testing of a flow visualization cell and a functional prototype. Major deliverables included: a determination of suitable electrode materials, an investigation of the destruction efficiency for numerous organic substrates, the construction and testing of a flow visualization cell, and the testing of a functional prototype commercial cell. The responsibilities of EOSystems included the definition of the market and potential customers, the design and engineering of the flow visualization and prototype cells, and the commercialization of the MEO units. Deliverables included the selection of the process and ancillary systems, the design of a flow visualization cell, and the design and construction of a prototype cell. In general, most of the deliverables were met by both partners, although unexpected technical difficulties delayed some of the delivery dates and forced the adoption of a modified statement of work. However, the primary, original project goals were completed on-time and on-budget.

  19. Degradation of conazole fungicides in water by electrochemical oxidation.

    PubMed

    Urzúa, J; González-Vargas, C; Sepúlveda, F; Ureta-Zañartu, M S; Salazar, R

    2013-11-01

    The electrochemical oxidation (EO) treatment in water of three conazole fungicides, myclobutanil, triadimefon and propiconazole, has been carried out at constant current using a BDD/SS system. First, solutions of each fungicide were electrolyzed to assess the effect of the experimental parameters such as current, pH and fungicide concentration on the decay of each compound and total organic carbon abatement. Then a careful analysis of the degradation by-products was made by high performance liquid chromatography, ion chromatography and gas chromatography coupled with mass spectrometry in order to provide a detailed discussion on the original reaction pathways. Thus, during the degradation of conazole fungicides by the electrochemical oxidation process, aromatic intermediates, aliphatic carboxylic acids and Cl(-) were detected prior to their complete mineralization to CO2 while NO3(-) anions remained in the treated solution. This is an essential preliminary step towards the applicability of the EO processes for the treatment of wastewater containing conazole fungicides. Copyright © 2013 Elsevier Ltd. All rights reserved.

  20. Selective electrochemical generation of hydrogen peroxide from water oxidation

    DOE PAGES

    Viswanathan, Venkatasubramanian; Hansen, Heine A.; Norskov, Jens K.

    2015-10-08

    Water is a life-giving source, fundamental to human existence, yet over a billion people lack access to clean drinking water. The present techniques for water treatment such as piped, treated water rely on time and resource intensive centralized solutions. In this work, we propose a decentralized device concept that can utilize sunlight to split water into hydrogen and hydrogen peroxide. The hydrogen peroxide can oxidize organics while the hydrogen bubbles out. In enabling this device, we require an electrocatalyst that can oxidize water while suppressing the thermodynamically favored oxygen evolution and form hydrogen peroxide. Using density functional theory calculations, wemore » show that the free energy of adsorbed OH* can be used to determine selectivity trends between the 2e– water oxidation to H2O2 and the 4e– oxidation to O2. We show that materials which bind oxygen intermediates sufficiently weakly, such as SnO2, can activate hydrogen peroxide evolution. Furthermore, we present a rational design principle for the selectivity in electrochemical water oxidation and identify new material candidates that could perform H2O2 evolution selectively.« less

  1. Selective electrochemical generation of hydrogen peroxide from water oxidation

    SciTech Connect

    Viswanathan, Venkatasubramanian; Hansen, Heine A.; Norskov, Jens K.

    2015-10-08

    Water is a life-giving source, fundamental to human existence, yet over a billion people lack access to clean drinking water. The present techniques for water treatment such as piped, treated water rely on time and resource intensive centralized solutions. In this work, we propose a decentralized device concept that can utilize sunlight to split water into hydrogen and hydrogen peroxide. The hydrogen peroxide can oxidize organics while the hydrogen bubbles out. In enabling this device, we require an electrocatalyst that can oxidize water while suppressing the thermodynamically favored oxygen evolution and form hydrogen peroxide. Using density functional theory calculations, we show that the free energy of adsorbed OH* can be used to determine selectivity trends between the 2e– water oxidation to H2O2 and the 4e– oxidation to O2. We show that materials which bind oxygen intermediates sufficiently weakly, such as SnO2, can activate hydrogen peroxide evolution. Furthermore, we present a rational design principle for the selectivity in electrochemical water oxidation and identify new material candidates that could perform H2O2 evolution selectively.

  2. Degradation of caffeine by conductive diamond electrochemical oxidation.

    PubMed

    Indermuhle, Chloe; Martín de Vidales, Maria J; Sáez, Cristina; Robles, José; Cañizares, Pablo; García-Reyes, Juan F; Molina-Díaz, Antonio; Comninellis, Christos; Rodrigo, Manuel A

    2013-11-01

    The use of Conductive-Diamond Electrochemical Oxidation (CDEO) and Sonoelectrochemical Oxidation (CDSEO) has been evaluated for the removal of caffeine of wastewater. Effects of initial concentration, current density and supporting electrolyte on the process efficiency are assessed. Results show that caffeine is very efficiently removed with CDEO and that depletion of caffeine has two stages depending on its concentration. At low concentrations, opposite to what it is expected in a mass-transfer controlled process, the efficiency increases with current density very significantly, suggesting a very important role of mediated oxidation processes on the removal of caffeine. In addition, the removal of caffeine is faster than TOC, indicating the formation of reaction intermediates. The number and relative abundance of them depend on the operating conditions and supporting electrolyte used. In chloride media, removal of caffeine is faster and more efficiently, although the occurrence of more intermediates takes place. CDSEO does not increase the efficiency of caffeine removal, but it affects to the formation of intermediates. A detailed characterization of intermediates by liquid chromatography time-of-flight mass spectrometry seems to indicate that the degradation of caffeine by CDEO follows an oxidation pathway similar to mechanism proposed by other advanced oxidation processes.

  3. Synthesis of reduced graphene oxide/thorn-like titanium dioxide nanofiber aerogels with enhanced electrochemical performance for supercapacitor.

    PubMed

    Kim, Tae-Woong; Park, Soo-Jin

    2017-01-15

    Reduced graphene oxide (rGO)/thorn-like TiO2 nanofiber (TTF) aerogels, or GTTF aerogels, with different TTF weight ratios were successfully prepared by electrospinning, silica etching and hydrothermal combination method. During the hydrothermal reaction, the rGO nanosheets and TTF self-assembled into three-dimensional (3D) interconnected networks, in which the TTF is loaded onto the rGO nanosheets. The electrochemical performance of the GTTF aerogels was assessed using cyclic voltammetry and galvanostatic charge-discharge measurements in a 1M aqueous Na2SO4 electrolyte. The TTF-to-rGO ratio of the aerogel material significantly affected the electrochemical performance of the aerogel electrodes, and the GTTF aerogels prepared with 20wt% TTF (denoted GTTF-20) exhibited excellent electrochemical performance. The maximum specific capacitance of this aerogel electrode was 178F/g at a current density of 1A/g. The GTTF-20 aerogel also exhibited good electrochemical stability with a capacitance degradation of less than 10% after 3000cycles. We can deduce that the electrochemical performance of the as-prepared aerogels may be enhanced by increasing the chemical interactions between rGO and TiO2. The results indicate that the GTTF aerogels show enormous potential for application in energy storage devices.

  4. METHOD FOR PREPARATION OF SINTERABLE BERYLLIUM OXIDE

    DOEpatents

    Sturm, B.J.

    1963-08-13

    High-purity beryllium oxide for nuclear reactor applications can be prepared by precipitation of beryllium oxalate monohydrate from aqueous solution at a temperature above 50 deg C and subsequent calcination of the precipitate. Improved purification with respect to metallic impurities is obtained, and the product beryllium oxide sinters reproducibly to a high density. (AEC)

  5. Mineralization of the biocide chloroxylenol by electrochemical advanced oxidation processes.

    PubMed

    Skoumal, Marcel; Arias, Conchita; Cabot, Pere Lluís; Centellas, Francesc; Garrido, José Antonio; Rodríguez, Rosa María; Brillas, Enric

    2008-04-01

    Electrochemical advanced oxidation processes (EAOPs) are environmentally friendly methods based on the destruction of organic pollutants in wastewaters with in situ electrogenerated hydroxyl radical. This species is formed in anodic oxidation (AO) from water oxidation at the anode and in indirect electro-oxidation methods like electro-Fenton (EF) and photoelectro-Fenton (PEF) also from reaction between catalytic Fe2+ and H2O2 continuously produced at the O2-diffusion cathode. The PEF method involves the irradiation of the treated solution with UVA light to enhance the photolysis of organics including Fe(III) complexes. In this work, the oxidation power of such EAOPs to decontaminate synthetic wastewaters of the biocide chloroxylenol (4-chloro-3,5-dimethylphenol) at pH 3.0 is comparatively examined with an undivided electrolytic cell containing a Pt or boron-doped diamond (BDD) anode and a stainless steel or O2-diffusion cathode. The initial chlorine is released as Cl(-) ion, which remains stable in the medium using Pt or is oxidized to Cl2 on BDD. The biocide solutions can be completely decontaminated using AO with a BDD anode, as well as PEF with a Pt or BDD anode. The PEF procedure with a BDD anode is the most powerful method leading to total mineralization in about 300 min, practically independent of current density. When current density rises, the degradation rate of processes increases, but they become less efficient due to the larger enhancement of waste reactions of oxidants. Chloroxylenol is much more rapidly removed in EF and PEF than in AO. 2,6-dimethylhydroquinone, 2,6-dimethyl-p-benzoquinone and 3,5-dimethyl-2-hydroxy-p-benzoquinone are identified as aromatic by-products, and maleic, malonic, pyruvic, acetic and oxalic acids are found as generated carboxylic acids. A general pathway for chloroxylenol mineralization by all EAOPs including the above by-products is proposed.

  6. Electrochemical performance of Sn-Sb-Cu film anodes prepared by layer-by-layer electrodeposition

    NASA Astrophysics Data System (ADS)

    Jiang, Qianlei; Xue, Ruisheng; Jia, Mengqiu

    2012-02-01

    A novel layer-by-layer electrodeposition and heat-treatment approach was attempted to obtain Sn-Sb-Cu film anode for lithium ion batteries. The preparation of Sn-Sb-Cu anodes started with galvanostatic electrochemically depositing antimony and tin sequentially on the substrate of copper foil collector. Sn-Sb and Cu-Sb alloys were formed when heated. The SEM analysis showed that the crystalline grains become bigger and the surface of the Sn-Sb-Cu anode becomes more denser after annealing. The energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) analysis showed the antimony, tin and copper were alloyed to form SnSb and Cu2Sb after heat treatment. The X-ray photoelectron spectroscopy (XPS) analysis showed the surface of the Sn-Sb-Cu electrode was covered by a thin oxide layer. Electrochemical measurements showed that the annealed Sn-Sb-Cu anode has high reversible capacity and good capacity retention. It exhibited a reversible capacity of about 962 mAh/g in the initial cycle, which still remained 715 mAh/g after 30 cycles.

  7. Morphology, structural and optical properties of iron oxide thin film photoanodes in photoelectrochemical cell: Effect of electrochemical oxidation

    NASA Astrophysics Data System (ADS)

    Maabong, Kelebogile; Machatine, Augusto G.; Hu, Yelin; Braun, Artur; Nambala, Fred J.; Diale, Mmantsae

    2016-01-01

    Hematite (α-Fe2O3) is a promising semiconductor as photoanode in solar hydrogen production from photoelectrolysis of water due to its appropriate band gap, low cost and high electrochemical stability in aqueous caustic electrolytes. Operation of such photoanode in a biased photoelectrochemical cell constitutes an anodization with consequent redox reactions at the electrode surface. α-Fe2O3 thin film photoanodes were prepared by simple and inexpensive dip coating method on fluorine doped tin oxide (FTO) glass substrate, annealed in air at 500 °C for 2 h, then electrochemically oxidized (anodized) in 1 M KOH at 500 mV for 1 min in dark and light conditions. Changes in structural properties and morphology of α-Fe2O3 nanoparticles films were investigated by XRD, Raman spectroscopy and a high resolution FE-SEM. The average grain size was observed to increase from 57 nm for pristine samples to 73 and 77 nm for anodized samples in dark and light respectively. Broadening and red shift in Raman spectra in anodized samples may be attributed to lattice expansion upon oxidation. The UV-visible measurements revealed enhanced absorption in the photoanodes after the treatment. The findings suggest that the anodization of the photoelectrode in a biased cell causes not only changes of the molecular structure at the surface, but also changes in the crystallographic structure which can be detected with x-ray diffractometry.

  8. Electrochemical production of hydrogen coupled with the oxidation of arsenite.

    PubMed

    Kim, Jungwon; Kwon, Daejung; Kim, Kitae; Hoffmann, Michael R

    2014-01-01

    The production of hydrogen accompanied by the simultaneous oxidation of arsenite (As(III)) was achieved using an electrochemical system that employed a BiOx-TiO2 semiconductor anode and a stainless steel (SS) cathode in the presence of sodium chloride (NaCl) electrolyte. The production of H2 was enhanced by the addition of As(III) during the course of water electrolysis. The synergistic effect of As(III) on H2 production can be explained in terms of (1) the scavenging of reactive chlorine species (RCS), which inhibit the production of H2 by competing with water molecules (or protons) for the electrons on the cathode, by As(III) and (2) the generation of protons, which are more favorably reduced on the cathode than water molecules, through the oxidation of As(III). The addition of 1.0 mM As(III) to the electrolyte at a constant cell voltage (E cell) of 3.0 V enhanced the production of H2 by 12% even though the cell current (I cell) was reduced by 5%. The net effect results in an increase in the energy efficiency (EE) for H2 production (ΔEE) by 17.5%. Furthermore, the value ΔEE, which depended on As(III) concentration, also depended on the applied E cell. For example, the ΔEE increased with increasing As(III) concentration in the micromolar range but decreased as a function of E cell. This is attributed to the fact that the reactions between RCS and As(III) are influenced by both RCS concentration depending on E cell and As(III) concentration in the solution. On the other hand, the ΔEE decreased with increasing As(III) concentration in the millimolar range due to the adsorption of As(V) generated from the oxidation of As(III) on the semiconductor anode. In comparison to the electrochemical oxidation of certain organic compounds (e.g., phenol, 4-chlorophenol, 2-chlorophenol, salicylic acid, catechol, maleic acid, oxalate, and urea), the ΔEE obtained during As(III) oxidation (17.5%) was higher than that observed during the oxidation of the above organic compounds

  9. Graphene oxide functionalized with silver@silica-polyethylene glycol hybrid nanoparticles for direct electrochemical detection of quercetin.

    PubMed

    Veerapandian, Murugan; Seo, Yeong-Tai; Yun, Kyusik; Lee, Min-Ho

    2014-08-15

    A direct electrochemical detection of quercetin based on functionalized graphene oxide modified on gold-printed circuit board chip was demonstrated in this study. Functionalized graphene oxide materials are prepared by the covalent reaction of graphene oxide with silver@silica-polyethylene glycol nanoparticles (~12.35nm). Functionalized graphene oxide electrode shows a well-defined voltammetric response in phosphate buffered saline and catalyzes the oxidation of quercetin to quinone without the need of an enzyme. Significantly, the functionalized graphene oxide modified electrode exhibited a higher sensitivity than pristine gold-printed circuit board and graphene oxide electrodes, a wide concentration range of 7.5 to 1040nM and detection limit of 3.57nM. Developed biosensor platform is selective toward quercetin in the presence of an interferent molecule. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Manipulating microstructures and electrical properties of carbon fiber/reduced graphene oxide/nickel composite textiles with electrochemical deposition techniques

    NASA Astrophysics Data System (ADS)

    Cheng, Wei-Liang; Zhao, Quan-Liang; Shi, Fei

    2017-04-01

    Since graphene and their composites play significant roles in the catalysts, energy storage, electronics and other fields, where electron transport is highly critical, here, we introduce reduced graphene oxide (RGO) interfaces in the carbon fiber (CF) networks for preparing a novel lightweight carbon fiber/reduced graphene oxide/nickel (CF-RGO-Ni) composite textile. Upon the charaterizations on the microscopic morphologies, electrical and magnetic properties, and density, the presence of RGO nanosheets and nickel nanoparticles would substantially influence the related physical properties in the resulting composite textiles. Furthermore, the key parameters, including RGO loading, deposition time, current density and annealing temperature of carbon matrices, have been studied to understand their effects on the electrochemical deposition of nickel nanoparticles. Implication of the results suggests that the RGO interface is a unique medium for essentially promoting the electrochemical deposition kinetics and active sites for growing nickel nanoparticles, which indicates a universal approach for preparing advanced lightweight composites with the presence of graphene naonstructures.

  11. Electrochemically Formed Ultrafine Metal Oxide Nanocatalysts for High-Performance Lithium–Oxygen Batteries

    SciTech Connect

    Liu, Bin; Yan, Pengfei; Xu, Wu; Zheng, Jianming; He, Yang; Luo, Langli; Bowden, Mark E.; Wang, Chong-Min; Zhang, Ji-Guang

    2016-08-10

    Lithium-oxygen (Li-O2) battery has an extremely high theoretical specific energy density as compared with conventional energy storage systems. However, practical application of Li-O2 battery system still faces significant challenges, especially its poor cyclability. In this work, we report a new approach to synthesis ultrafine metal oxide nanocatalysts through an electrochemical pre-lithiation process. This process reduces the size of NiCo2O4 (NCO) particles from 20~30 nm to a uniformly distributed domain of ~ 2 nm and largely improved their catalytic activity. Structurally, the pre-lithiated NCO NWs are featured by ultrafine NiO/CoO nanoparticles, which show high stability during prolonged cycles in terms of morphology and the particle size, therefore maintaining an excellent catalytic effect to oxygen reduction and evolution reactions. Li-O2 battery using this catalyst has demonstrated an initial capacity of 29,280 mAh g-1 and has retained a stable capacity of over 1,000 mAh g-1 after 100 cycles based on the weight of NCO active material. Direct in-situ TEM observation conclusively reveals the lithiation/delithiation process of as-prepared NCO NWs, clarifying the NCO/Li electrochemical reaction mechanism that can be extended to other transition-metal oxides and providing the in depth understandings on the catalysts and battery chemistries of other ternary transition-metal oxides.

  12. Electrochemical determination of estradiol using a thin film containing reduced graphene oxide and dihexadecylphosphate.

    PubMed

    Janegitz, Bruno C; dos Santos, Fabrício A; Faria, Ronaldo C; Zucolotto, Valtencir

    2014-04-01

    Graphene is a material that has attracted attention with regard to sensing and biosensing applications in recent years. Here, we report a novel treatment (using ultrasonic bath and ultrasonic tip) to obtain graphene oxide (GO) and a new stable conducting film using reduced graphene oxide (RGO) and dihexadecylphosphate film (DHP). The GO was obtained by chemical exfoliation and it was reduced using NaBH4. Subsequently, RGO-DHP dispersion was prepared and it was dropped onto a glassy carbon electrode by casting technique. The electrode was characterized by cyclic voltammetry and electrochemical spectroscopy impedance. The voltammetric behavior of the RGO-DHP/GC electrode in the presence of estradiol was studied, and the results reported an irreversible oxidation peak current at 0.6V. Under the optimal experimental conditions, using linear sweep adsorptive stripping voltammetry, the detection limit obtained for this hormone was 7.7×10(-8)mol L(-1). The proposed electrode can be attractive for applications as electrochemical sensors and biosensors.

  13. A simple preparation of graphite/gelatin composite for electrochemical detection of dopamine.

    PubMed

    Rajkumar, Chellakannu; Thirumalraj, Balamurugan; Chen, Shen-Ming; Chen, His-An

    2017-02-01

    In this study, we demonstrate a simple preparation of graphite (GR) sheets assisted with gelatin (GLN) polypeptide composite was developed for sensitive detection of dopamine (DA) sensor. The GR/GLN composite was prepared by GR powder in GLN solution (5mg/mL) via sonication process. The prepared GR/GLN composite displays well dispersion ability in biopolymer matrix and characterized via scanning electron microscope (SEM), Fourier transform infrared (FTIR) spectroscopy and electrochemical impedance spectroscopy (EIS) studies. The GR/GLN modified electrode showed an excellent electrocatalytic activity toward the oxidation of DA, suggesting that the successful formation of GR sheets crosslinked with the functional groups of GLN polypeptide. In addition, the GR/GLN modified electrode achieved a wide linear response ranging from 0.05 to 79.5μM with a detection limit of 0.0045μM. The calculated analytical sensitivity of the sensor was 1.36±0.02μAμM(-1)cm(-2). Conversely, the modified electrode demonstrates a good storage stability, reproducibility and repeatability. In addition, the sensor manifests the determination of DA in human serum and urine samples for practical applications. Copyright © 2016 Elsevier Inc. All rights reserved.

  14. Optical and electrochemical properties of Cu-doped NiO films prepared by electrochemical deposition

    NASA Astrophysics Data System (ADS)

    Zhao, Lili; Su, Ge; Liu, Wei; Cao, Lixin; Wang, Jing; Dong, Zheng; Song, Meiqin

    2011-02-01

    Cu-doped nickel oxide (NiO) thin films were prepared by electrochemial deposition (cathodic deposition) technique onto the fluorine doped tin oxide (F: SnO2; FTO) coated glass substrates from organic solutions. Effects of Cu content on the morphology, structure, optical and electrochromic properties of NiO films were investigated by means of scanning electron microscope (SEM), X-ray diffraction (XRD), ultraviolet-visible spectrophotometer (UV-vis) and cyclic voltammetry (CV), respectively. SEM images indicated the formation of nanorods after Cu was added. The films were formed with amorphous or short-range ordered NiO grains and a trace of face-centered cubic NixCu1-xO confirmed by XRD. The transmittances of both bleached state and colored state were significantly lowered when Cu was added. The NiO films doped with Cu (the molar ratio was 1/8) exhibited the optimum electrochromic behavior with a variation of transmittance (ΔT) up to ∼80% at the wavelength range of 350-600 nm. Cu doping reduces the response time for both the coloring and bleaching states, and the reversibility of the redox reaction was increased as well.

  15. Cuprous Sulfide/Reduced Graphene Oxide Hybrid Nanomaterials: Solvothermal Synthesis and Enhanced Electrochemical Performance

    NASA Astrophysics Data System (ADS)

    He, Zhanjun; Zhu, Yabo; Xing, Zheng; Wang, Zhengyuan

    2016-01-01

    The cuprous sulfide nanoparticles (CuS NPs)-decorated reduced graphene oxide (rGO) nanocomposites have been successfully prepared via a facile and efficient solvothermal synthesis method. Scanning electron microscopy and transmission electron microscopy images demonstrated that CuS micronspheres composed of nanosheets and distributed on the rGO layer in well-monodispersed form. Fourier-transform infrared spectroscopy analyses and x-ray photoelectron spectroscopy showed that graphene oxide (GO) had been reduced to rGO. The electrochemical performances of CuS/rGO nanocomposites were investigated by cyclic voltammetry and charge/discharge techniques, which showed that the specific capacitance of CuS/rGO nanocomposites was enhanced because of the introduction of rGO.

  16. Electrochemical oxidation for the treatment of textile industry wastewater.

    PubMed

    Radha, K V; Sridevi, V; Kalaivani, K

    2009-01-01

    This study elucidates the reduction of organics from textile effluents through electrochemical oxidation technique. Effect of pH and current intensity were investigated in this system. It was found that degradation was maximum at the current intensity of 0.6 A and at a pH of 1.3. Under the same experimental conditions the removal of chemical oxygen demand (COD), total solids, total dissolved solids and total organic carbon were found to be approximately 68%, 49.2%, 50.7% and 96.8%, respectively. Effect of current intensity on color removal was also investigated as a function of electrolysis time (30-210 minutes) and it showed that maximum removal efficiency (96%) was reached within 60 minutes at 0.6 A. While studying the effect of pH on COD removal, it was observed that a decrease in pH to an optimum of 1.3 showed maximum COD reduction of 68%. These results suggest an important role of these parameters in electrochemical process for removing organic pollutants.

  17. Electrochemical oxidation and reuse of tannery saline wastewater.

    PubMed

    Sundarapandiyan, S; Chandrasekar, R; Ramanaiah, B; Krishnan, S; Saravanan, P

    2010-08-15

    In this present work, electrochemical treatment of saline wastewater with organic (protein) load was studied. The influence of the critical parameters of electro-oxidation such as pH, period, salt concentration and current density on the reduction of organic load was studied using graphite electrodes. It was found that current density of 0.024 A/cm(2) for a period of 2 h at pH 9.0 rendered best results in terms of reduction in COD and TKN. The energy requirement for the reduction of 1 kg of TKN and 1 kg of COD are 22.45 kWh and 0.80 kWh respectively at pH 9 and 0.024 A/cm(2). Reuse experiments were conducted at commercial scale. One of the saline waste streams in leather manufacturing process, pickling was treated and reused continuously thrice. The characteristics of the waste stream and the quality of the leathers indicate that the reuse of saline streams with intermittent electrochemical treatment is feasible.

  18. Electrochemical Oxidation of EDTA in Nuclear Wastewater Using Platinum Supported on Activated Carbon Fibers

    PubMed Central

    Zhao, Bo; Zhu, Wenkun; Mu, Tao; Hu, Zuowen; Duan, Tao

    2017-01-01

    A novel Pt/ACF (Pt supported on activated carbon fibers) electrode was successfully prepared with impregnation and electrodeposition method. Characterization of the electrodes indicated that the Pt/ACF electrode had a larger effective area and more active sites. Electrochemical degradation of ethylenediaminetetra-acetic acid (EDTA) in aqueous solution with Pt/ACF electrodes was investigated. The results showed that the 3% Pt/ACF electrode had a better effect on EDTA removal. The operational parameters influencing the electrochemical degradation of EDTA with 3% Pt/ACF electrode were optimized and the optimal removal of EDTA and chemical oxygen demand (COD) were 94% and 60% after 100 min on condition of the electrolyte concentration, initial concentration of EDTA, current density and initial value of pH were 0.1 mol/L, 300 mg/L, 40 mA/cm2 and 5.0, respectively. The degradation intermediates of EDTA in electrochemical oxidation with 3% Pt/ACF electrode were identified by gas chromatography-mass spectrum (GC-MS). PMID:28754016

  19. Zinc oxide nanowires-based electrochemical biosensor for L-lactic acid amperometric detection

    NASA Astrophysics Data System (ADS)

    Zhao, Yanguang; Yan, Xiaoqin; Kang, Zhuo; Fang, Xiaofei; Zheng, Xin; Zhao, Lanqing; Du, Hongwu; Zhang, Yue

    2014-05-01

    In this work, zinc oxide (ZnO) nanowires-based electrochemical biosensor is designed and fabricated for the detection of L-lactic acid. ZnO nanowires were successfully synthesized via the chemical vapor deposition method. The morphology and structure of the prepared products were characterized, and the average diameter of synthesized ZnO samples was 500 nm. The fluorescence characterization was performed to verify the immobilization of lactate oxidase onto the ZnO surface. Biosensors based on large-area ZnO nanowires were then constructed, and a series of electrochemical experiments showed that ZnO could provide the efficient electron transfer channel between the enzymic active sites and the electrode surface. The proposed electrochemical biosensor exhibited a sensitivity of 15.6 µA cm-2 mM-1, a wide linear range of 12 µM-1.2 mM with a low-detection limit of 12 µM for L-lactic acid detection. This study has indicated the potential applications for ZnO nanowires to construct the simple and economic nano-bio devices for the detection of biological species.

  20. Decolourisation of simulated reactive dyebath effluents by electrochemical oxidation assisted by UV light.

    PubMed

    López-Grimau, V; Gutiérrez, M C

    2006-01-01

    This study is focused on the optimisation of the electrochemical decolourisation of textile effluents containing reactive dyes with the aim of making feasible-technically and economically-this method at industrial scale. Coloured waters were treated in continuous at low current density, to reduce the electrical consumption. Ti/PtO(x) electrodes were used to oxidize simulated dyebaths prepared with an azo/dichlorotriazine reactive dye (C.I. Reactive Orange 4). The decolourisation yield was dependent on the dyeing electrolyte (NaCl or Na(2)SO(4)). Dyeing effluents which contained from 0.5 to 20 gl(-1) of NaCl reached a high decolourisation yield, depending on the current density, immediately after the electrochemical process. These results were improved when the effluents were stored for several hours under solar light. After the electrochemical treatment the effluents were stored in a tank and exposed under different lighting conditions: UV light, solar light and darkness. The evolution of the decolourisation versus the time of storage was reported and kinetic constants were calculated. The time of storage was significantly reduced by the application of UV light. A dye mineralization study was also carried out on a concentrated dyebath. A TOC removal of 81% was obtained when high current density was applied for a prolonged treatment with recirculation. This treatment required a high electrical consumption.

  1. Enhanced photocatalytic activity of electrochemically synthesized aluminum oxide nanoparticles

    NASA Astrophysics Data System (ADS)

    Pathania, Deepak; Katwal, Rishu; Kaur, Harpreet

    2016-03-01

    In this study, aluminum oxide (Al2O3) nanoparticles (NPs) were synthesized via an electrochemical method. The effects of reaction parameters such as supporting electrolytes, solvent, current and electrolysis time on the shape and size of the resulting NPs were investigated. The Al2O3 NPs were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, transmission electron microscopy, thermogravimetric analysis/differential thermal analysis, energy-dispersive X-ray analysis, and ultraviolet-visible spectroscopy. Moreover, the Al2O3 NPs were explored for photocatalytic degradation of malachite green (MG) dye under sunlight irradiation via two processes: adsorption followed by photocatalysis; coupled adsorption and photocatalysis. The coupled process exhibited a higher photodegradation efficiency (45%) compared to adsorption followed by photocatalysis (32%). The obtained kinetic data was well fitted using a pseudo-first-order model for MG degradation.

  2. Research Update: Nanoscale electrochemical transistors in correlated oxides

    NASA Astrophysics Data System (ADS)

    Kanki, Teruo; Tanaka, Hidekazu

    2017-04-01

    Large reversible changes of the electronic transport properties of solid-state oxide materials induced by electrochemical fields have received much attention as a new research avenue in iontronics. In this research update, dramatic transport changes in vanadium dioxide (VO2) nanowires were demonstrated by electric field-induced hydrogenation at room temperature through the nanogaps separated by humid air in a field-effect transistor structure with planar-type gates. This unique structure allowed us to investigate hydrogen intercalation and diffusion behavior in VO2 channels with respect to both time and space. Our results will contribute to further strategic researches to examine fundamental chemical and physical properties of devices and develop iontronic applications, as well as offering new directions to explore emerging functions for sensing, energy, and neuromorphologic devices combining ionic and electronic behaviors in solid-state materials.

  3. Preliminary studies using hybrid mediated electrochemical oxidation (HMEO) for the removal of persistent organic pollutants (POPs).

    PubMed

    Chung, S J; Balaji, S; Matheswaran, M; Ramesh, T; Moon, I S

    2007-01-01

    This study investigates the hybrid mediated electrochemical oxidation (HMEO) technology, which is a newly developed non thermal electrochemical oxidation process for organic destruction. A combination of ozone and ultrasonication processes to the mediated electrochemical oxidation (MEO) process is termed as hybrid mediated electrochemical oxidation. The electrochemical cell was developed in this laboratory. In the present study, several organic compounds, such as phenol, benzoquinone and ethylenediaminetetraacetic acid (EDTA), were chosen as the model organic pollutants to be destructed by the hybrid process. The organic destruction was monitored based on the CO2 generation and total organic carbon (TOC) reduction. The HMEO process was found to be extremely effective in the destruction of all the target organics chosen in this study. The information obtained from this study will provide an insight in adopting this technique for dealing with more recalcitrant organics (POPs).

  4. Vanadium oxides nanostructures: Hydrothermal synthesis and electrochemical properties

    SciTech Connect

    Mjejri, I.; Etteyeb, N.; Sediri, F.

    2014-12-15

    Highlights: • Vanadium oxides nanostructures were synthesized hydrothermally. • Reversible redox behavior with doping/dedoping process. • Doping/dedoping is easier for Li{sup +} to Na{sup +}. • Energy-related applications such as cathodes in lithium batteries. - Abstract: A facile and template-free one-pot strategy is applied to synthesize nanostructured vanadium oxide particles via a hydrothermal methodology. X-ray diffraction (XRD), scanning electron microscope (SEM), Fourier transforms infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) have been used to characterize the structure and morphology of the samples. The products are gradually changed from sheet-shaped VO{sub 2}(B) to rod-like V{sub 3}O{sub 7}·H{sub 2}O with decreasing cyclohexanediol as both protective and reducing agent. The specific surface area of the VO{sub 2}(B) nanosheets and V{sub 3}O{sub 7}·H{sub 2}O nanorods was found to be 22 and 16 m{sup 2} g{sup −1}, respectively. Thin films of VO{sub 2}(B) and V{sub 3}O{sub 7}·H{sub 2}O deposited on ITO substrates were electrochemically characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The voltammograms show reversible redox behavior with doping/dedoping process corresponding to reversible cation intercalation/de-intercalation into the crystal lattice of the nanorods/nanosheets. This process is easier for the small Li{sup +} cation than larger ones Na{sup +}.

  5. Morphological and electrochemical properties of crystalline praseodymium oxide nanorods.

    PubMed

    Shamshi Hassan, M; Shaheer Akhtar, M; Shim, Kyung-Bo; Yang, O-Bong

    2010-02-05

    Highly crystalline Pr6O11 nanorods were prepared by a simple precipitation method of triethylamine complex at 500°C. Synthesized Pr6O11 nanorods were uniformly grown with the diameter of 12-15 nm and the length of 100-150 nm without any impurities of unstable PrO2 phase. The Pr6O11 nanorod electrodes attained a high electrical conductivity of 0.954 Scm-1 with low activation energy of 0.594 eV at 850°C. The electrochemical impedance study showed that the resistance of electrode was significantly decreased at high temperature, which resulted from its high conductivity and low activation energy. The reduced impedance and high electrical conductivity of Pr6O11 nanorod electrodes are attributed to the reduction of grain boundaries and high space charge width.

  6. Electrochemical Deposition of Iron Nanoneedles on Titanium Oxide Nanotubes

    SciTech Connect

    Gan Y. X.; Zhang L.; Gan B.J.

    2011-10-01

    Iron as a catalyst has wide applications for hydrogen generation from ammonia, photodecomposition of organics, and carbon nanotube growth. Tuning the size and shape of iron is meaningful for improving the catalysis efficiency. It is the objective of this work to prepare nanostructured iron with high surface area via electrochemical deposition. Iron nanoneedles were successfully electrodeposited on Ti supported TiO2 nanotube arrays in a chlorine-based electrolyte containing 0.15 M FeCl2 {center_dot} 4H2O and 2.0 M HCl. Transmission electron microscopic analysis reveals that the average length of the nanoneedles is about 200 nm and the thickness is about 10 nm. It has been found that a high overpotential at the cathode made of Ti/TiO2 nanotube arrays is necessary for the formation of the nanoneedles. Cyclic voltammetry test indicates that the electrodeposition of iron nanoneedles is a concentration-limited process.

  7. Preparation of activated carbon from wet sludge by electrochemical-NaClO activation.

    PubMed

    Miao, Chen; Ye, Caihong; Zhu, Tianxing; Lou, Ziyang; Yuan, Haiping; Zhu, Nanwen

    2014-01-01

    Activated carbon (AC) from sludge is one potential solution for sewage sludge disposal, while the drying sludge is cost and time consuming for preparation. AC preparation from the wet sludge with electrochemical-NaClO activation was studied in this work. Three pretreatment processes, i.e. chemical activation, electrolysis and electrochemical-reagent reaction, were introduced to improve the sludge-derived AC properties, and the optimum dosage of reagent was tested from the 0.1:1 to 1:1 (mass rate, reagent:dried sludge). It was shown that the electrochemical-NaClO preparation is the best method under the test conditions, in which AC has the maximum Brunauer, Emmett and Teller area of 436 m²/g at a mass ratio of 0.7. Extracellular polymeric substances in sludge can be disintegrated by electrochemical-NaClO pretreatment, with a disintegration degree of more than 45%. The percentage of carbon decreased from 34.16 to 8.81 after treated by electrochemical-NaClO activation. Fourier transform infrared spectra showed that a strong C-Cl stretching was formed in electrochemical-NaClO prepared AC. The maximum adsorption capacity of AC reaches 109 mg/g on MB adsorption experiment at pH 10 and can be repeated for three times with high removal efficiency after regeneration.

  8. Electrochemical performance of a solid oxide fuel cell with an anode based on Cu-Ni/CeO2 for methane direct oxidation

    NASA Astrophysics Data System (ADS)

    Hornés, Aitor; Escudero, María J.; Daza, Loreto; Martínez-Arias, Arturo

    2014-03-01

    A CuNi-CeO2/YSZ/LSF solid oxide fuel cell has been fabricated and tested with respect to its electrochemical activity for direct oxidation of dry methane. The electrodes have been prepared by impregnation of corresponding porous YSZ layers, using reverse microemulsions as impregnating medium for the anode (constituted by Cu-Ni at 1:1 atomic ratio in combination with CeO2). On the basis of I-V electrochemical testing complemented by impedance spectroscopy (IS) measurements it is shown the ability of the SOFC for direct oxidation of methane in a rather stable way. Differences in the behavior as a function of operating temperature (1023-1073 K) are also revealed and examined on the basis of analysis of IS spectra.

  9. Ruthenium Oxide-Based Microelectrochemical Devices: Electrochemical Behavior of the Oxide Formed by Reduction of RuO4(2-)

    DTIC Science & Technology

    1988-08-15

    579 I i1. TITLE (include Security Classification) Ruthemium Oxide-Based Microelectrochemical Devices : Electrochem. _Behavior of the Oxide Formed by...Ruthenium Oxide-Based Microelectrochemical Devices : Electrochemical Behavior of the Oxide Formed by Reduction of RuO4 2- by Djonald F. Lyons, Martin 0...RUTHENIUM OXIDE-BASED MICROELECTROCHEMICAL DEVICES : ELECTROCHEMICAL BEHAVIOR OF THE OXIDE FORMED BY REDUCTION OF Ruo4 2- Donald F. Lyons, Martin 0

  10. Electrochemical study on the adsorption of carbon oxides and oxidation of their adsorption products on platinum group metals and alloys.

    PubMed

    Siwek, Hanna; Lukaszewski, Mariusz; Czerwiński, Andrzej

    2008-07-07

    CO(2) reduction and CO adsorption on noble metals (Pt, Rh, Pd) and their alloys (Pt-Rh, Pd-Pt, Pd-Rh, Pd-Pt-Rh) prepared as thin rough deposits have been studied by chronoamperometry (CA), cyclic voltammetry (CV) and the electrochemical quartz crystal microbalance (EQCM). The influence of alloy surface composition on the values of surface coverage, eps (electron per site) and potential of the oxidation of CO(2) reduction and CO adsorption products is shown. The oxidation of the adsorbate on Pt-Rh alloys proceeds more easily (at lower potentials) than on pure metals. On the other hand, in the case of Pd-Pt and Pd-Rh alloys the adsorbate oxidation is more difficult and requires higher potentials than on Pt or Rh. The analysis of the EQCM signal is presented for the case of adsorption and oxidation of carbon oxide adsorption products on the electrodes studied. The comparison of adsorption parameters and the EQCM response obtained for platinum group metals and alloys leads to the conclusion that reduced CO(2) cannot be totally identified with adsorbed CO.

  11. Preparation and characterization of STM tips for electrochemical studies

    NASA Astrophysics Data System (ADS)

    Nagahara, L. A.; Thundat, T.; Lindsay, S. M.

    1989-10-01

    We report on a fabrication technique for scanning tunneling microscopy (STM) tips for in situ electrochemical investigations. Unwanted Faradaic currents were minimized by insulating the STM tips with Apiezon wax. Cyclic voltammetry showed Apiezon wax to be inert in various electrolytes.

  12. Preparation of polyphenols by oxidation of hydroxybenzaldehydes

    SciTech Connect

    Formanek, K.; Michelet, D.; Petre, D.

    1984-03-06

    Optionally aldehyde substituted polyphenols are prepared by oxidizing, with hydrogen peroxide, a hydroxybenzaldehyde bearing at least one aldehyde substituent ortho- and/or para- to the nuclear hydroxyl group, in an aqueous reaction medium and in the presence of an alkali or alkaline earth metal base, the process being characterized in that the pH of the reaction medium is continuously maintained at a value no greater than 7 throughout the course of the oxidation reaction. The subject process is well suited for the preparation of, e.g., hydroxy-p-vanillin from guaiacol, and the novel compound 2,4,6-triformylphenol.

  13. Process for preparing active oxide powders

    DOEpatents

    Berard, Michael F.; Hunter, Jr., Orville; Shiers, Loren E.; Dole, Stephen L.; Scheidecker, Ralph W.

    1979-02-20

    An improved process for preparing active oxide powders in which cation hydroxide gels, prepared in the conventional manner are chemically dried by alternately washing the gels with a liquid organic compound having polar characteristics and a liquid organic compound having nonpolar characteristics until the mechanical water is removed from the gel. The water-free cation hydroxide is then contacted with a final liquid organic wash to remove the previous organic wash and speed drying. The dried hydroxide treated in the conventional manner will form a highly sinterable active oxide powder.

  14. Coimmobilization of urease and glutamate dehydrogenase in electrochemically prepared polypyrrole-polyvinyl sulfonate films.

    PubMed

    Gambhir, A; Gerard, M; Mulchandani, A K; Malhotra, B D

    2001-01-01

    Immobilization of urease and glutamate dehydrogenase enzymes in electrochemically prepared polypyrrole-polyvinyl sulfonate films (PPY-PVS) was carried out using physical adsorption and electrochemical entrapment techniques. Detailed studies on optimum pH, Fourier transform infrared spectroscopy, cyclic voltammetry, and scanning electron microscopy of the enzymes in the immobilized state were conducted. The value of the apparent Michaelis-Menten constant was experimentally determined to be 2.5 and 2.7 for physically adsorbed and electrochemically entrapped urease in PPY-PVS films, respectively.

  15. A reduced graphene oxide based electrochemical biosensor for tyrosine detection

    NASA Astrophysics Data System (ADS)

    Wei, Junhua; Qiu, Jingjing; Li, Li; Ren, Liqiang; Zhang, Xianwen; Chaudhuri, Jharna; Wang, Shiren

    2012-08-01

    In this paper, a ‘green’ and safe hydrothermal method has been used to reduce graphene oxide and produce hemin modified graphene nanosheet (HGN) based electrochemical biosensors for the determination of l-tyrosine levels. The as-fabricated HGN biosensors were characterized by UV-visible absorption spectra, fluorescence spectra, Fourier transform infrared spectroscopy (FTIR) spectra and thermogravimetric analysis (TGA). The experimental results indicated that hemin was successfully immobilized on the reduced graphene oxide nanosheet (rGO) through π-π interaction. TEM images and EDX results further confirmed the attachment of hemin on the rGO nanosheet. Cyclic voltammetry tests were carried out for the bare glass carbon electrode (GCE), the rGO electrode (rGO/GCE), and the hemin-rGO electrode (HGN/GCE). The HGN/GCE based biosensor exhibits a tyrosine detection linear range from 5 × 10-7 M to 2 × 10-5 M with a detection limitation of 7.5 × 10-8 M at a signal-to-noise ratio of 3. The sensitivity of this biosensor is 133 times higher than that of the bare GCE. In comparison with other works, electroactive biosensors are easily fabricated, easily controlled and cost-effective. Moreover, the hemin-rGO based biosensors demonstrate higher stability, a broader detection linear range and better detection sensitivity. Study of the oxidation scheme reveals that the rGO enhances the electron transfer between the electrode and the hemin, and the existence of hemin groups effectively electrocatalyzes the oxidation of tyrosine. This study contributes to a widespread clinical application of nanomaterial based biosensor devices with a broader detection linear range, improved stability, enhanced sensitivity and reduced costs.

  16. A reduced graphene oxide based electrochemical biosensor for tyrosine detection.

    PubMed

    Wei, Junhua; Qiu, Jingjing; Li, Li; Ren, Liqiang; Zhang, Xianwen; Chaudhuri, Jharna; Wang, Shiren

    2012-08-24

    In this paper, a 'green' and safe hydrothermal method has been used to reduce graphene oxide and produce hemin modified graphene nanosheet (HGN) based electrochemical biosensors for the determination of l-tyrosine levels. The as-fabricated HGN biosensors were characterized by UV-visible absorption spectra, fluorescence spectra, Fourier transform infrared spectroscopy (FTIR) spectra and thermogravimetric analysis (TGA). The experimental results indicated that hemin was successfully immobilized on the reduced graphene oxide nanosheet (rGO) through π-π interaction. TEM images and EDX results further confirmed the attachment of hemin on the rGO nanosheet. Cyclic voltammetry tests were carried out for the bare glass carbon electrode (GCE), the rGO electrode (rGO/GCE), and the hemin-rGO electrode (HGN/GCE). The HGN/GCE based biosensor exhibits a tyrosine detection linear range from 5 × 10(-7) M to 2 × 10(-5) M with a detection limitation of 7.5 × 10(-8) M at a signal-to-noise ratio of 3. The sensitivity of this biosensor is 133 times higher than that of the bare GCE. In comparison with other works, electroactive biosensors are easily fabricated, easily controlled and cost-effective. Moreover, the hemin-rGO based biosensors demonstrate higher stability, a broader detection linear range and better detection sensitivity. Study of the oxidation scheme reveals that the rGO enhances the electron transfer between the electrode and the hemin, and the existence of hemin groups effectively electrocatalyzes the oxidation of tyrosine. This study contributes to a widespread clinical application of nanomaterial based biosensor devices with a broader detection linear range, improved stability, enhanced sensitivity and reduced costs.

  17. Electrochemical Synthesis of Polypyrrole, Reduced Graphene Oxide, and Gold Nanoparticles Composite and Its Application to Hydrogen Peroxide Biosensor

    PubMed Central

    Wu, Baoyan; Zhao, Na; Hou, Shihua; Zhang, Cong

    2016-01-01

    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. PMID:28335348

  18. Electrochemical Synthesis of Polypyrrole, Reduced Graphene Oxide, and Gold Nanoparticles Composite and Its Application to Hydrogen Peroxide Biosensor.

    PubMed

    Wu, Baoyan; Zhao, Na; Hou, Shihua; Zhang, Cong

    2016-11-21

    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 (Au(3+)) 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.

  19. Amine functionalized graphene oxide/CNT nanocomposite for ultrasensitive electrochemical detection of trinitrotoluene.

    PubMed

    Sablok, Kavita; Bhalla, Vijayender; Sharma, Priyanka; Kaushal, Roohi; Chaudhary, Shilpa; Suri, C Raman

    2013-03-15

    Binding of electron-deficient trinitrotoluene (TNT) to the electron rich amine groups on a substrate form specific charge-transfer Jackson-Meisenheimer (JM) complex. In the present work, we report formation of specific JM complex on amine functionalized reduced graphene oxide/carbon nanotubes- (a-rGO/CNT) nanocomposite leading to sensitive detection of TNT. The CNT were dispersed using graphene oxide that provides excellent dispersion by attaching to CNT through its hydrophobic domains and solubilizes through the available OH and COOH groups on screen printed electrode (SPE). The GO was reduced electrochemically to form reduced graphene that remarkably increases electrochemical properties owing to the intercalation of high aspect CNT on graphene flakes as shown by TEM micrograph. The surface amine functionalization of dropcasted and rGO/CNT was carried out using a bi-functional cross linker ethylenediamine. The extent of amine functionalization on modified electrodes was confirmed using energy dispersive X-ray (EDX), X-ray photoelectron spectroscopy (XPS) and confocal microscopy. The FTIR and Raman spectra further suggested the formation of JM complex between amine functionalized electrodes and TNT leading to a shift in peak intensity together with peak broadening. The a-rGO/CNT nanocomposite prepared electrode surface leads to ultra-trace detection of TNT upto 0.01 ppb with good reproducibility (n=3). The a-rGO/CNT sensing platform could be an alternate for sensitive detection of TNT explosive for various security and environmental applications.

  20. Electrochemically Formed Ultrafine Metal Oxide Nanocatalysts for High-Performance Lithium-Oxygen Batteries.

    PubMed

    Liu, Bin; Yan, Pengfei; Xu, Wu; Zheng, Jianming; He, Yang; Luo, Langli; Bowden, Mark E; Wang, Chong-Min; Zhang, Ji-Guang

    2016-08-10

    Lithium-oxygen (Li-O2) batteries have an extremely high theoretical specific energy density when compared with conventional energy-storage systems. However, practical application of the Li-O2 battery system still faces significant challenges. In this work, we report a new approach for synthesis of ultrafine metal oxide nanocatalysts through an electrochemical prelithiation process. This process reduces the size of NiCo2O4 (NCO) particles from 20-30 nm to a uniformly distributed domain of ∼2 nm and significantly improves their catalytic activity. Structurally, the prelithiated NCO nanowires feature ultrafine NiO/CoO nanoparticles that are highly stable during prolonged cycles in terms of morphology and particle size, thus maintaining an excellent catalytic effect to oxygen reduction and evolution reactions. A Li-O2 battery using this catalyst demonstrated an initial capacity of 29 280 mAh g(-1) and retained a capacity of >1000 mAh g(-1) after 100 cycles based on the weight of the NCO active material. Direct in situ transmission electron microscopy observations conclusively revealed the lithiation/delithiation process of as-prepared NCO nanowires and provided in-depth understanding for both catalyst and battery chemistries of transition-metal oxides. This unique electrochemical approach could also be used to form ultrafine nanoparticles of a broad range of materials for catalyst and other applications.

  1. High-throughput synthesis and electrochemical screening of a library of modified electrodes for NADH oxidation.

    PubMed

    Pinczewska, Aleksandra; Sosna, Maciej; Bloodworth, Sally; Kilburn, Jeremy D; Bartlett, Philip N

    2012-10-31

    We report the combinatorial preparation and high-throughput screening of a library of modified electrodes designed to catalyze the oxidation of NADH. Sixty glassy carbon electrodes were covalently modified with ruthenium(II) or zinc(II) complexes bearing the redox active 1,10-phenanthroline-5,6-dione (phendione) ligand by electrochemical functionalization using one of four different linkers, followed by attachment of one of five different phendione metal complexes using combinatorial solid-phase synthesis methodology. This gave a library with three replicates of each of 20 different electrode modifications. This library was electrochemically screened in high-throughput (HTP) mode using cyclic voltammetry. The members of the library were evaluated with regard to the surface coverage, midpeak potential, and voltammetric peak separation for the phendione ligand, and their catalytic activity toward NADH oxidation. The surface coverage was found to depend on the length and flexibility of the linker and the geometry of the metal complex. The choices of linker and metal complex were also found to have significant impact on the kinetics of the reaction between the 1,10-phenanthroline-5,6-dione ligand and NADH. The rate constants for the reaction were obtained by analyzing the catalytic currents as a function of NADH concentration and scan rate, and the influence of the surface molecular architecture on the kinetics was evaluated.

  2. Effect of hydrothermal reaction time and alkaline conditions on the electrochemical properties of reduced graphene oxide

    NASA Astrophysics Data System (ADS)

    Vermisoglou, E. C.; Giannakopoulou, T.; Romanos, G.; Giannouri, M.; Boukos, N.; Lei, C.; Lekakou, C.; Trapalis, C.

    2015-12-01

    Reduced graphene oxide sheets (rGO) were prepared by hydrothermal treatment of aqueous dispersions of graphite oxide (GtO) applied for short (4 h) and prolonged reaction times (19-24 h). The effect of process duration as well as the alkaline conditions (pH ∼10) by addition of K2CO3 on the quality characteristics of the produced rGO materials was investigated. Both reduction and exfoliation occurred during this process as it was evidenced by FTIR and XRD data. SEM, TEM and HRTEM microscopy displayed highly exfoliated rGO materials. XPS verified that the re-establishment of the conjugated graphene network is more extensive for prolonged times of hydrothermal processing in accordance to Raman spectroscopy measurements. The sample produced under alkaline conditions bore fewer defects and almost 5 times higher BET surface area (∼181 m2/g) than the sample with no pH adjustment (∼34 m2/g) for the same hydrothermal reaction time (19 h), attributed to the developed microporosity. The specific capacitance of this material estimated by electrochemical impedance using three-electrode cell and KCl aqueous solution as an electrolyte was ∼400-500 F/g. When EDLC capacitors were fabricated from rGO materials the electrochemical testing in organic electrolyte i.e. TEABF4 in PC, revealed that the shortest hydrothermal reaction time (4 h) was more efficient resulting in capacitance around 60 F/g.

  3. Electrochemical, H2O2-Boosted Catalytic Oxidation System

    NASA Technical Reports Server (NTRS)

    Akse, James R.; Thompson, John O.; Schussel, Leonard J.

    2004-01-01

    An improved water-sterilizing aqueous-phase catalytic oxidation system (APCOS) is based partly on the electrochemical generation of hydrogen peroxide (H2O2). This H2O2-boosted system offers significant improvements over prior dissolved-oxygen water-sterilizing systems in the way in which it increases oxidation capabilities, supplies H2O2 when needed, reduces the total organic carbon (TOC) content of treated water to a low level, consumes less energy than prior systems do, reduces the risk of contamination, and costs less to operate. This system was developed as a variant of part of an improved waste-management subsystem of the life-support system of a spacecraft. Going beyond its original intended purpose, it offers the advantage of being able to produce H2O2 on demand for surface sterilization and/or decontamination: this is a major advantage inasmuch as the benign byproducts of this H2O2 system, unlike those of systems that utilize other chemical sterilants, place no additional burden of containment control on other spacecraft air- or water-reclamation systems.

  4. Treatment and toxicity evaluation of methylene blue using electrochemical oxidation, fly ash adsorption and combined electrochemical oxidation-fly ash adsorption.

    PubMed

    Wang, Kai-sung; Wei, Ming-Chi; Peng, Tzu-Huan; Li, Heng-Ching; Chao, Shu-Ju; Hsu, Tzu-Fang; Lee, Hong-Shen; Chang, Shih-Hsien

    2010-08-01

    Treatment of a basic dye, methylene blue, by electrochemical oxidation, fly ash adsorption, and combined electrochemical oxidation-fly ash adsorption was compared. Methylene blue at 100 mgL(-1) was used in this study. The toxicity was also monitored by the Vibrio fischeri light inhibition test. When electrochemical oxidation was used, 99% color and 84% COD were removed from the methylene blue solution in 20 min at a current density of 428 Am(-2), NaCl of 1000 mgL(-1), and pH(0) of 7. However, the decolorized solution showed high toxicity (100% light inhibition). For fly ash adsorption, a high dose of fly ash (>20,000 mgL(-1)) was needed to remove methylene blue, and the Freundlich isotherm described the adsorption behavior well. In the combined electrochemical oxidation-fly ash adsorption treatment, the addition of 4000 mgL(-1) fly ash effectively reduced intermediate toxicity and decreased the COD of the electrochemical oxidation-treated methylene blue solution. The results indicated that the combined process effectively removed color, COD, and intermediate toxicity of the methylene blue solution.

  5. Improved electrochemical biosensor response via metal oxide pre-oxidation of chemical interferents

    NASA Astrophysics Data System (ADS)

    Houseknecht, Jamie G.; Tapsak, Mark A.

    2007-09-01

    Typical biological samples are inherently complicated. They may contain a myriad of compounds that are electroactive at the same potential as that used in many electrochemical biosensors. Therefore, a biosensor design feature must be included that either eliminates or blocks the interferents from generating false positive signals. The ability to use an insoluble compound, that of MnO II, in order to oxidize interferents such as ascorbic acid, acetaminophen and uric acid, was investigated in a prototype sensor system at a bias potential of 0.6 V versus Ag/AgCl. Unlike previous work with these materials, a difference between the ability for the metal oxide to oxidize the interferents was observed. Most effective was the capability of MnO II to oxidize uric acid. Alternatively, the MnO II had little effect on acetaminophen. The study is both introduced and results are discussed within the context of an implantable glucose sensor.

  6. Demonstration of Electrochemical Cell Properties by a Simple, Colorful Oxidation-reduction Experiment.

    ERIC Educational Resources Information Center

    Hendricks, Lloyd J.; And Others

    1982-01-01

    Describes apparatus/methodology and provides background information for an experiment demonstrating electrochemical concepts and properties of electrochemical cells. The color of a solution close to an electrode is changed from that of the bulk solution to either of two contrasting colors depending on whether the reaction is oxidation or…

  7. Bone reactions to oxidized titanium implants with electrochemical anion sulphuric acid and phosphoric acid incorporation.

    PubMed

    Sul, Young-Taeg; Johansson, Carina B; Kang, Yunmo; Jeon, Dong-Gyun; Albrektsson, Tomas

    2002-01-01

    The importance of the surface properties of implants for a successful osseointegration has been emphasized. It is generally known that bone response to implant surfaces is considerably related to the various surface properties. The purpose of this study was to investigate bone tissue reactions to multifactorial biocompatibility of the surface oxide of electrochemically oxidized titanium implants. The ultimate objective was to improve surface quality, resulting in enhancement of clinical outcomes of osseointegrated implants. Three different surface types of commercially pure titanium (c.p. Ti) implants were prepared. Turned implants were used for controls and test implants were prepared by the micro arc oxidation (MAO) method, either in sulphuric acid (S implants) or in phosphoric acid (P implants). Implants were inserted in the femur and tibia of 10 mature New Zealand White rabbits. The bone response was evaluated by biomechanical tests, histology, and histomorphometry. The follow-up time was 6 weeks. The mean peak values of the removal torque showed significant differences between control and test S implants (p =.022) but showed no significant differences between control and test P implants (p =.195) or between test S and test P implants (p =.457). In addition, the histomorphometric comparisons of the bone-to-metal contact around entire implants demonstrated 186% increase in S implants (p =.028) and 232% increase in P implants (p =.028) compared with the paired control groups. Quantification of the bone area in the threads did not show any significant differences. The present results suggest that the primary mode of action in strong bone response to S implants is mechanical interlocking, and to P implants, it is biochemical interaction. It is possible that the phosphate groups in the titanium oxide of P implants provide potential chemical bonding sites for calcium ions and hydroxyapatite of the bone matrix during biologic mineralization. key words: bone responses

  8. Fe3O4 magnetic nanoparticles/reduced graphene oxide nanosheets as a novel electrochemical and bioeletrochemical sensing platform.

    PubMed

    Teymourian, Hazhir; Salimi, Abdollah; Khezrian, Somayeh

    2013-11-15

    We have developed Fe3O4 magnetic nanoparticles/reduced graphene oxide nanosheets modified glassy carbon (Fe3O4/r-GO/GC) electrode as a novel system for the preparation of electrochemical sensing platform. Decorating Fe3O4 nanoparticles on graphene sheets was performed via a facile one-step chemical reaction strategy, where the reduction of GO and the in-situ generation of Fe3O4 nanoparticles occurred simultaneously. Characterization of as-made nanocomposite using X-ray diffraction (XRD), transmission electron microscopy (TEM) and alternative gradient force magnetometry (AGFM) clearly demonstrate the successful attachment of monodisperse Fe3O4 nanoparticles to graphene sheets. Electrochemical studies revealed that the Fe3O4/r-GO/GC electrode possess excellent electrocatalytic activities toward the low potential oxidation of NADH (0.05 V vs. Ag/AgCl) as well as the catalytic reduction of O2 and H2O2 at reduced overpotentials. Via immobilization of lactate dehydrogenase (LDH) as a model dehydrogenase enzyme onto the Fe3O4/r-GO/GC electrode surface, the ability of modified electrode for biosensing lactate was demonstrated. In addition, using differential pulse voltammetry (DPV) to investigate the electrochemical oxidation behavior of ascorbic acid (AA), dopamine (DA) and uric acid (UA) at Fe3O4/r-GO/GC electrode, the high electrocatalytic activity of the modified electrode toward simultaneous detection of these compounds was indicated. Finally, based on the strong electrocatalytic action of Fe3O4/r-GO/GC electrode toward both oxidation and reduction of nitrite, a sensitive amperometric sensor for nitrite determination was proposed. The Fe3O4/r-GO hybrid presented here showing favorable electrochemical features may hold great promise to the development of electrochemical sensors, molecular bioelectronic devices, biosensors and biofuel cells.

  9. Electrochemical preparation and delivery of melanin-iron covered gold nanoparticles.

    PubMed

    Grumelli, Doris; Vericat, Carolina; Benítez, Guillermo; Ramallo-López, José M; Giovanetti, Lisandro; Requejo, Félix; Moreno, M Sergio; Orive, Alejandro González; Creus, Alberto Hernández; Salvarezza, Roberto C

    2009-02-02

    Attractive combination: Biopolymer-modified nanoparticles which combine magnetic properties with biocompatibility are prepared and delivered following a three-step strategy (see figure): i) Adsorption of thiol-capped metal nanoparticles on graphite, ii) electrochemical modification, iii) potential-induced delivery of the modified nanoparticles to the electrolyte. Thiol-capped gold nanoparticles modified with iron-melanin are attractive because they combine magnetic properties and biocompatibility. The biopolymer modified nanoparticles are prepared and delivered following a three step strategy: i) adsorption of thiol-capped metal nanoparticles on graphite, ii) electrochemical deposition of melanin-iron, iii) potential-induced delivery of the modified nanoparticles to the electrolyte.

  10. Costs of the electrochemical oxidation of wastewaters: a comparison with ozonation and Fenton oxidation processes.

    PubMed

    Cañizares, Pablo; Paz, Rubén; Sáez, Cristina; Rodrigo, Manuel A

    2009-01-01

    In the work described here the technical and economic feasibilities of three Advanced Oxidation Processes (AOPs) have been studied: Conductive-Diamond Electrochemical Oxidation (CDEO), Ozonation and Fenton oxidation. The comparison was made by assessing the three technologies with synthetic wastewaters polluted with different types of organic compounds and also with actual wastes (from olive oil mills and from a fine-chemical manufacturing plant). All three technologies were able to treat the wastes, but very different results were obtained in terms of efficiency and mineralization. Only CDEO could achieve complete mineralization of the pollutants for all the wastes. However, the efficiencies were found to depend on the concentration of pollutant (mass transfer control of the oxidation rate). Results obtained in the oxidation with ozone (at pH 12) or by Fenton's reagent were found to depend on the nature of the pollutants, and significant concentrations of oxidation-refractory compounds were usually accumulated during the treatment. Within the discharge limits that all of the technologies can reach, the economic analysis shows that the operating cost of Fenton oxidation is lower than either CDEO or ozonation, although CD\\EO can compete satisfactorily with the Fenton process in the treatment of several kinds of wastes. Likewise, the investment cost for the ozonation process seems to be higher than either CDEO or Fenton oxidation, regardless of the pollutant treated.

  11. Electrochemically reduced graphene and iridium oxide nanoparticles for inhibition-based angiotensin-converting enzyme inhibitor detection.

    PubMed

    Kurbanoglu, Sevinc; Rivas, Lourdes; Ozkan, Sibel A; Merkoçi, Arben

    2017-02-15

    In this work, a novel biosensor based on electrochemically reduced graphene oxide and iridium oxide nanoparticles for the detection of angiotensin-converting enzyme inhibitor drug, captopril, is presented. For the preparation of the biosensor, tyrosinase is immobilized onto screen printed electrode by using 1-Ethyl-3-(3-dimethylaminopropyl)-carbodiimide and N-Hydroxysuccinimide coupling reagents, in electrochemically reduced graphene oxide and iridium oxide nanoparticles matrix. Biosensor response is characterized towards catechol, in terms of graphene oxide concentration, number of cycles to reduce graphene oxide, volume of iridium oxide nanoparticles and tyrosinase solution. The designed biosensor is used to inhibit tyrosinase activity by Captopril, which is generally used to treat congestive heart failure. It is an angiotensin-converting enzyme inhibitor that operates via chelating copper at the active site of tyrosinase and thioquinone formation. The captopril detections using both inhibition ways are very sensitive with low limits of detection: 0.019µM and 0.008µM for chelating copper at the active site of tyrosinase and thioquinone formation, respectively. The proposed methods have been successfully applied in captopril determination in spiked human serum and pharmaceutical dosage forms with acceptable recovery values. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Electrochemical deposition of high density gold nanoparticles on indium/tin oxide electrode for fabrication of biosensors.

    PubMed

    Yu, Xiuping; Wang, Liping; Di, Junwei

    2011-12-01

    High density gold nanoparticles (GNPs) on indium tin oxide (ITO) film coated glass have been prepared by one-step electrochemical deposition from KAu(CN)2 in phosphate buffer (pH 8.0) solution. The resulting electrode surface was characterized by scanning electron microscopy (SEM), UV-vis spectroscopy, X-ray diffraction (XRD) and electrochemical method. Experimental results revealed that the number density of the nanoparticles was increased by the negative shift of the applied potential, while the coverage of the deposited GNPs on ITO substrate surface was also increased by means of the increasing deposition cycles. The presence of GNPs with high coverage improved the electrochemical response of Fe(CN)6 (3-/4-). This high coverage GNP/ITO substrate was applied to immobilization superoxide dismutase (SOD) for fabrication of electrochemical biosensors. The direct electron transfer between enzyme and electrode was realized, and the electrochemical performance of the SOD electrode was improved with the high coverage of GNPs. The biosensor exhibited a rapid and high response to superoxide anion.

  13. Electrochemical properties of iodine-containing lithium manganese oxide spinel

    NASA Astrophysics Data System (ADS)

    Han, Chi-Hwan; Hong, Young-Sik; Hong, Hyun-Sil; Kim, Keon

    Iodine-containing, cation-deficient, lithium manganese oxides (ICCD-LMO) are prepared by reaction of MnO 2 with LiI. The MnO 2 is completely transformed into spinel-structured compounds with a nominal composition of Li 1- δMn 2-2 δO 4I x. A sample prepared at 800 °C, viz. Li 0.99Mn 1.98O 4I 0.02, exhibits an initial discharge capacity of 113 mA h g -1 with good cycleability and rate capability in the 4-V region. Iodine-containing, lithium-rich lithium manganese oxides (ICLR-LMO) are also prepared by reaction of LiMn 2O 4 with LiI, which results in a nominal composition of Li 1+ xMn 2- xO 4I x. Li 1.01Mn 1.99O 4I 0.02 shows a discharge capacity of 124 mA h g -1 on the first cycle and 119 mA h g -1 a on the 20th cycle. Both results indicate that a small amount of iodine species helps to maintain cycle performance.

  14. Electrochemical oxidation of reverse osmosis concentrate on mixed metal oxide (MMO) titanium coated electrodes.

    PubMed

    Bagastyo, Arseto Y; Radjenovic, Jelena; Mu, Yang; Rozendal, René A; Batstone, Damien J; Rabaey, Korneel

    2011-10-15

    Reverse osmosis (RO) membranes have been successfully applied around the world for wastewater reuse applications. However, RO is a physical separation process, and besides the clean water stream (permeate) a reverse osmosis concentrate (ROC) is produced, usually representing 15-25% of the feed water flow and containing the organic and inorganic contaminants at higher concentrations. In this study, electrochemical oxidation was investigated for the treatment of ROC generated during the reclamation of municipal wastewater effluent. Using laboratory-scale two-compartment electrochemical systems, five electrode materials (i.e. titanium coated with IrO2-Ta2O5, RuO2-IrO2, Pt-IrO2, PbO2, and SnO2-Sb) were tested as anodes in batch mode experiments, using ROC from an advanced water treatment plant. The best oxidation performance was observed for Ti/Pt-IrO2 anodes, followed by the Ti/SnO2-Sb and Ti/PbO2 anodes. The effectiveness of the treatment appears to correlate with the formation of oxidants such as active chlorine (i.e. Cl2/HClO/ClO-). As a result, electro-generated chlorine led to the abundant formation of harmful by-products such as trihalomethanes (THMs) and haloacetic acids (HAAs), particularly at Ti/SnO2-Sb and Ti/Pt-IrO2 anodes. The highest concentration of total HAAs (i.e. 2.7 mg L(-1)) was measured for the Ti/SnO2-Sb electrode, after 0.55 Ah L(-1) of supplied specific electrical charge. Irrespective of the used material, electrochemical oxidation of ROC needs to be complemented by a polishing treatment to alleviate the release of halogenated by-products. Copyright © 2011 Elsevier Ltd. All rights reserved.

  15. Comparative electrochemical analysis of crystalline and amorphous anodized iron oxide nanotube layers as negative electrode for LIB.

    PubMed

    Pervez, Syed Atif; Kim, Doohun; Farooq, Umer; Yaqub, Adnan; Choi, Jung-Hee; Lee, You-Jin; Doh, Chil-Hoon

    2014-07-23

    This work is a comparative study of the electrochemical performance of crystalline and amorphous anodic iron oxide nanotube layers. These nanotube layers were grown directly on top of an iron current collector with a vertical orientation via a simple one-step synthesis. The crystalline structures were obtained by heat treating the as-prepared (amorphous) iron oxide nanotube layers in ambient air environment. A detailed morphological and compositional characterization of the resultant materials was performed via transmission electron microscopy (TEM), field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), and Raman spectroscopy. The XRD patterns were further analyzed using Rietveld refinements to gain in-depth information on their quantitative phase and crystal structures after heat treatment. The results demonstrated that the crystalline iron oxide nanotube layers exhibit better electrochemical properties than the amorphous iron oxide nanotube layers when evaluated in terms of the areal capacity, rate capability, and cycling performance. Such an improved electrochemical response was attributed to the morphology and three-dimensional framework of the crystalline nanotube layers offering short, multidirectional transport lengths, which favor rapid Li(+) ions diffusivity and electron transport.

  16. Electrochemical preparation of hexanitrostilbene (HNS) from hexanitrobibenzyl (HNBB). [Hexanitrostilbene (HNS)

    SciTech Connect

    Firsich, D.W.

    1986-09-17

    The development of an electrochemical synthesis for the explosive hexanitrostilbene (HNS) from hexanitrobibenzyl (HNBB) is described. A tertiary amine first removes two protons from HNBB; the resulting dianionic species is then electrolyzed at an inert electrode to produce HNS. The characterization of the chemistry and electrochemistry in this transformation is presented, and the properties of the species involved are compared with those of related molecules. Liquid Chromatography shows that the above synthetic procedure produces HNS with no observed side products and in virtually quantitative yield. The potential for scale-up to a manufacturing process is discussed. 19 refs., 6 figs.

  17. Electrochemical capacitor performance of hydrous ruthenium oxide/mesoporous carbon composite electrodes

    NASA Astrophysics Data System (ADS)

    Jang, Jong H.; Han, Sangjin; Hyeon, Taeghwan; Oh, Seung M.

    Ruthenium/carbon composite materials are prepared by impregnating ruthenium(III) acetylacetonate into a mesoporous carbon (average pore diameter=12 mn, pore volume=3.6 cm 3 g -1) and then heat treatment at 320 °C for 2 h under an argon atmosphere. The metallic ruthenium nanoparticles are converted to pseudo-capacitive hydrous ruthenium oxide by electrochemical oxidation at 0.75 V (versus SCE) for 2 h in 2.0 M H 2SO 4. The specific capacitance of the composite electrodes, which is the sum of the double-layer capacitance of mesoporous carbon and the pseudo-capacitance of hydrous ruthenium oxide, reaches 243 F g -1 with heavy loading. As the loading is increased, however, the degree of ruthenium utilization for a pseudo-capacitor becomes poorer, presumably due to a limited conversion to the hydrous oxide form. The rate capability of composite electrodes also decreases with increase in ruthenium loading, due to an increase in both the equivalent series resistance (ESR) and the overall capacitance value. The ESR enlargement is caused mainly an increase in the electrolyte resistance within pores which, in turn, results from a pore narrowing with ruthenium loading Hindered ionic motion in narrowed pores can explain this feature. An increase in the RC time constant with ruthenium loading is further verified by ac impedance measurements.

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

    NASA Astrophysics Data System (ADS)

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

    2017-05-01

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

  19. Electrochemically Reduced Graphene Oxide Multilayer Films as Efficient Counter Electrode for Dye-Sensitized Solar Cells

    PubMed Central

    Xu, Xiaobao; Huang, Dekang; Cao, Kun; Wang, Mingkui; Zakeeruddin, Shaik M.; Grätzel, Michael

    2013-01-01

    We report on a new counter electrode for dye-sensitized solar cells (DSCs), which is prepared using layer-by-layer assembly of negatively charged graphene oxide and positively charged poly (diallyldimethylammonium chloride) followed by an electrochemical reduction procedure. The DSC devises using the heteroleptic Ru complex C106TBA as sensitizer and this new counter electrode reach power conversion efficiencies of 9.5% and 7.6% in conjunction with low volatility and solvent free ionic liquid electrolytes, respectively. The new counter electrode exhibits good durability (60°C for 1000 h in a solar simulator, 100 mW cm−2) during the accelerated tests when used in combination with an ionic liquid electrolyte. This work identifies a new class of electro-catalysts with potential for low cost photovoltaic devices. PMID:23508212

  20. Electrochemical oxidation of methanol on Pt nanoparticles composited MnO 2 nanowire arrayed electrode

    NASA Astrophysics Data System (ADS)

    Zhao, Guang-Yu; Li, Hu-Lin

    2008-03-01

    By use of the membrane-template synthesis route, MnO 2 nanowire arrayed electrodes are successfully synthesized by means of the anodic deposition technique. The Pt nanoparticles composited MnO 2 nanowire arrayed electrodes (PME) are obtained through depositing Pt on MnO 2 nanowire arrayed electrode by cathode deposition technique. For comparison of electrochemical performance, Pt nanowire arrayed electrodes which have the same amount of Pt with PME are also prepared. The electro-oxidation of methanol on PME and Pt nanowire arrayed electrodes is investigated at room temperature by cyclic voltammetry, which show that about 110 mV decreased overpotential and 2.1-fold enhanced votammetric current are achieved on PME. The chronoamperometry result demonstrates that the resistance to carbon monoxide for PME is improved.

  1. Electrochemically active, anti-biofouling polymer adlayers on indium-tin-oxide electrodes.

    PubMed

    Kim, Eun Jeong; Shin, Hee-Young; Park, Sangjin; Sung, Daekyung; Jon, Sangyong; Sampathkumar, Srinivasa-Gopalan; Yarema, Kevin J; Choi, Sung-Yool; Kim, Kyuwon

    2008-08-14

    Here we report the synthesis of a novel electrochemically active polymer, preparation of adlayers of the polymer on optically transparent electrodes, and an application of the adlayers to immobilization of engineered cells through a direct covalent coupling reaction.

  2. Eliminating degradation in solid oxide electrochemical cells by reversible operation.

    PubMed

    Graves, Christopher; Ebbesen, Sune Dalgaard; Jensen, Søren Højgaard; Simonsen, Søren Bredmose; Mogensen, Mogens Bjerg

    2015-02-01

    One promising energy storage technology is the solid oxide electrochemical cell (SOC), which can both store electricity as chemical fuels (electrolysis mode) and convert fuels to electricity (fuel-cell mode). The widespread use of SOCs has been hindered by insufficient long-term stability, in particular at high current densities. Here we demonstrate that severe electrolysis-induced degradation, which was previously believed to be irreversible, can be completely eliminated by reversibly cycling between electrolysis and fuel-cell modes, similar to a rechargeable battery. Performing steam electrolysis continuously at high current density (1 A cm(-2)), initially at 1.33 V (97% energy efficiency), led to severe microstructure deterioration near the oxygen-electrode/electrolyte interface and a corresponding large increase in ohmic resistance. After 4,000 h of reversible cycling, however, no microstructural damage was observed and the ohmic resistance even slightly improved. The results demonstrate the viability of applying SOCs for renewable electricity storage at previously unattainable reaction rates, and have implications for our fundamental understanding of degradation mechanisms that are usually assumed to be irreversible.

  3. Electrochemical oxidation of textile industry wastewater by graphite electrodes.

    PubMed

    Bhatnagar, Rajendra; Joshi, Himanshu; Mall, Indra D; Srivastava, Vimal C

    2014-01-01

    In the present article, studies have been performed on the electrochemical (EC) oxidation of actual textile industry wastewater by graphite electrodes. Multi-response optimization of four independent parameters namely initial pH (pHo): 4-10, current density (j): 27.78-138.89 A/m(2), NaCl concentration (w): 0-2 g/L and electrolysis time (t): 10-130 min have been performed using Box-Behnken (BB) experimental design. It was aimed to simultaneously maximize the chemical oxygen demand (COD) and color removal efficiencies and minimize specific energy consumption using desirability function approach. Pareto analysis of variance (ANOVA) showed a high coefficient of determination value for COD (R(2) = 0.8418), color (R(2) = 0.7010) and specific energy (R(2) = 0.9125) between the experimental values and the predicted values by a second-order regression model. Maximum COD and color removal and minimum specific energy consumed was 90.78%, 96.27% and 23.58 kWh/kg COD removed, respectively, were observed at optimum conditions. The wastewater, sludge and scum obtained after treatment at optimum condition have been characterized by various techniques. UV-visible study showed that all azo bonds of the dyes present in the wastewater were totally broken and most of the aromatic rings were mineralized during EC oxidation with graphite electrode. Carbon balance showed that out of the total carbon eroded from the graphite electrodes, 27-29.2% goes to the scum, 71.1-73.3% goes into the sludge and rest goes to the treated wastewater. Thermogravimetric analysis showed that the generated sludge and scum can be dried and used as a fuel in the boilers/incinerators.

  4. Facile and controllable electrochemical reduction of graphene oxide and its applications

    SciTech Connect

    Shao, Yuyan; Wang, Jun; Engelhard, Mark H.; Wang, Chong M.; Lin, Yuehe

    2010-01-01

    Graphene oxide is electrochemically reduced which is called electrochemically reduced graphene oxide (ER-G). ER-G is characterized with scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, and X-ray diffraction. The oxygen content is significantly decreased and the sp 2 carbon is restored after electrochemical reduction. ER-G exhibits much higher electrochemical capacitance and cycling durability than carbon nanotubes (CNTs) and chemically reduced graphene; the specific capacitance measured with cyclic voltammetry (20 mV/s) is ~165 F/g, ~86 F/g, and ~100 F/g for ER-G, CNTs, and chemically reduced graphene,1 respectively. The electrochemical reduction of oxygen and hydrogen peroxide was greatly enhanced on ER-G electrodes as compared with CNTs. ER-G has shown a good potential for applications in energy storage, biosensors, and electrocatalysis.

  5. Boron-doped cadmium oxide composite structures and their electrochemical measurements

    SciTech Connect

    Lokhande, B.J.; Ambare, R.C.; Mane, R.S.; Bharadwaj, S.R.

    2013-08-01

    Graphical abstract: Conducting nano-fibrous 3% boron doped cadmium oxide thin films were prepared by SILAR and its super capacitive properties were studied. - Highlights: • Samples are of nanofibrous nature. • All samples shows pseudocapacitive behavior. • 3% B doped CdO shows good specific capacitance. • 3% B doped CdO shows maximum 74.93% efficiency at 14 mA/cm{sup 2}. • 3% B doped CdO shows 0.8 Ω internal resistance. - Abstract: Boron-doped and undoped cadmium oxide composite nanostructures in thin film form were prepared onto stainless steel substrates by a successive ionic layer adsorption and reaction method using aqueous solutions of cadmium nitrate, boric acid and 1% H{sub 2}O{sub 2}. As-deposited films were annealed at 623 K for 1 h. The X-ray diffraction study shows crystalline behavior for both doped and undoped films with a porous topography and nano-wires type architecture, as observed in SEM image. Wettability test confirms the hydrophilic surface with 58° contact angle value. Estimated band gap energy is around 1.9 eV. Electrochemical behavior of the deposited films is attempted in 1 M KOH electrolyte using cyclic voltammetry (CV), electrochemical impedance spectroscopy and galvanostatic charge–discharge tests. Maximum values of the specific capacitance, specific energy and specific power obtained for 3% B doped CdO film at 2 mV/s scan rate are 20.05 F/g, 1.22 Wh/kg and 3.25 kW/kg, respectively.

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

    PubMed

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

    2017-07-15

    In this research, the electrochemical biosensor composed of myoglobin (Mb) on molybdenum disulfide nanoparticles (MoS2 NP) encapsulated with graphene oxide (GO) was fabricated for the detection of hydrogen peroxide (H2O2). Hybrid structure composed of MoS2 NP and GO (GO@MoS2) was fabricated for the first time to enhance the electrochemical signal of the biosensor. As a sensing material, Mb was introduced to fabricate the biosensor for H2O2 detection. Formation and immobilization of GO@MoS2 was confirmed by transmission electron microscopy, ultraviolet-visible spectroscopy, scanning electron microscopy, and scanning tunneling microscopy. Immobilization of Mb, and electrochemical property of biosensor were investigated by cyclic voltammetry and amperometric i-t measurements. Fabricated biosensor showed the electrochemical signal enhanced redox current as -1.86μA at an oxidation potential and 1.95μA at a reduction potential that were enhanced relative to those of electrode prepared without GO@MoS2. Also, this biosensor showed the reproducibility of electrochemical signal, and retained the property until 9 days from fabrication. Upon addition of H2O2, the biosensor showed enhanced amperometric response current with selectivity relative to that of the biosensor prepared without GO@MoS2. This novel hybrid material-based biosensor can suggest a milestone in the development of a highly sensitive detecting platform for biosensor fabrication with highly sensitive detection of target molecules other than H2O2.

  7. Solid-phase electrochemical reduction of graphene oxide films in alkaline solution.

    PubMed

    Basirun, Wan J; Sookhakian, Mehran; Baradaran, Saeid; Mahmoudian, Mohammad R; Ebadi, Mehdi

    2013-09-24

    Graphene oxide (GO) film was evaporated onto graphite and used as an electrode to produce electrochemically reduced graphene oxide (ERGO) films by electrochemical reduction in 6 M KOH solution through voltammetric cycling. Fourier transformed infrared and Raman spectroscopy confirmed the presence of ERGO. Electrochemical impedance spectroscopy characterization of ERGO and GO films in ferrocyanide/ferricyanide redox couple with 0.1 M KCl supporting electrolyte gave results that are in accordance with previous reports. Based on the EIS results, ERGO shows higher capacitance and lower charge transfer resistance compared to GO.

  8. Solid-phase electrochemical reduction of graphene oxide films in alkaline solution

    PubMed Central

    2013-01-01

    Graphene oxide (GO) film was evaporated onto graphite and used as an electrode to produce electrochemically reduced graphene oxide (ERGO) films by electrochemical reduction in 6 M KOH solution through voltammetric cycling. Fourier transformed infrared and Raman spectroscopy confirmed the presence of ERGO. Electrochemical impedance spectroscopy characterization of ERGO and GO films in ferrocyanide/ferricyanide redox couple with 0.1 M KCl supporting electrolyte gave results that are in accordance with previous reports. Based on the EIS results, ERGO shows higher capacitance and lower charge transfer resistance compared to GO. PMID:24059434

  9. Solid-phase electrochemical reduction of graphene oxide films in alkaline solution

    NASA Astrophysics Data System (ADS)

    Basirun, Wan J.; Sookhakian, Mehran; Baradaran, Saeid; Mahmoudian, Mohammad R.; Ebadi, Mehdi

    2013-09-01

    Graphene oxide (GO) film was evaporated onto graphite and used as an electrode to produce electrochemically reduced graphene oxide (ERGO) films by electrochemical reduction in 6 M KOH solution through voltammetric cycling. Fourier transformed infrared and Raman spectroscopy confirmed the presence of ERGO. Electrochemical impedance spectroscopy characterization of ERGO and GO films in ferrocyanide/ferricyanide redox couple with 0.1 M KCl supporting electrolyte gave results that are in accordance with previous reports. Based on the EIS results, ERGO shows higher capacitance and lower charge transfer resistance compared to GO.

  10. Electrochemical corrosion of a noble metal-bearing alloy-oxide composite

    DOE PAGES

    Chen, X; Ebert, W. L.; Indacochea, Ernesto

    2017-08-01

    The effects of added Ru and Pd on the microstructure and electrochemical behaviour of a composite material made by melting those metals with AISI 410 stainless steel, Zr, Mo, and lanthanide oxides were assessed using electrochemical and microscopic methods The lanthanide oxides reacted with Zr to form durable lanthanide zirconates and Mo alloyed with steel to form FeMoCr intermetallics. The noble metals alloyed with the steel to provide solid solution strengthening and inhibit carbide/nitride formation. A passive film formed during electrochemical tests in acidic NaCl solution, but became less effective as corrosion progressed and regions over the intermetallics eventually failed.

  11. Electrochemical lithium intercalation chemistry of condensed molybdenum metal cluster oxide: LiMo4O6

    NASA Astrophysics Data System (ADS)

    Lim, Sung-Chul; Chae, Munseok S.; Heo, Jongwook W.; Hong, Seung-Tae

    2017-10-01

    The electrochemical lithium-ion intercalation properties of molybdenum metal-cluster oxide LixMo4O6 (0.33 ≤ x ≤ 1.0) in an organic electrolyte of 1.0 M LiPF6 in ethylene carbonate/dimethyl carbonate (1:2 v/v) were characterized for the first time. Li0.66Mo4O6 (tetragonal, P4/mbm, a = 9.5914(3) Å, c = 2.8798(1) Å, V = 264.927(15) Å3, Z = 2) was prepared via ion-exchange of indium and lithium ions from InMo4O6 (tetragonal, P4/mbm, a = 9.66610(4) Å, c = 2.86507(2) Å, V = 267.694(2) Å3, Z = 2), which was first synthesized from a stoichiometric mixture of In, Mo, and MoO3 via a solid-state reaction for 11 h at 1100 °C. Then, Li0.33Mo4O6 was obtained via electrochemical charge of the electrode at 3.4 V vs. Li. The electrochemical lithium-ion insertion into Li0.33Mo4O6 occurs stepwise: three separate peaks were observed in the cyclic voltammogram and three quasi-plateaus in the galvanostatic profile, indicating a complicated intercalation mechanism. However, examination of the structural evolution of LixMo4O6 during the electrochemical cycle indicated a reversible reaction over the measured voltage range (2.0-3.2 V) and x range (0.33 ≤ x ≤ 1.00). Despite the excellent electrochemical reversibility, LixMo4O6 showed poor rate performance with a low capacity of 36.3 mAh g-1 at a rate of 0.05 C. Nonetheless, this work demonstrates a new structural class of lithium cathode materials with condensed metal clusters and 1D tunnels, and provides a host material candidate for multivalent-ion batteries.

  12. Nickel nanoparticles with hcp structure: Preparation, deposition as thin films and application as electrochemical sensor.

    PubMed

    Neiva, Eduardo G C; Oliveira, Marcela M; Marcolino, Luiz H; Zarbin, Aldo J G

    2016-04-15

    Hexagonal close packed (hcp) nickel nanoparticles stabilized by polyvinylpyrrolidone (PVP) were synthesized through the thermal treatment of face centered cubic (fcc) nickel nanoparticles. Controlling both the temperature of the heat treatment and the amount of PVP was possible the control of the hcp/fcc rate in the samples, where the higher Ni/PVP ratio produces only the hcp-nickel phase (average size of 8.9 nm) highly stable in air. The crystalline structure, the presence of PVP, the size of the nanoparticles and the stability of the hcp-nickel were confirmed using X-ray diffractometry, Fourier transform infrared spectroscopy, transmission electron microscopy, Raman spectroscopy, scanning electron microscopy and thermogravimetric analysis. Thin films of hcp and fcc nickel nanoparticles were prepared through a biphasic system and deposited over indium-doped tin oxide (ITO) substrates, which were electrochemically characterized and applied as glycerol amperometric sensors in NaOH medium. Parameters as the number of cycles applied and the scan rate were evaluated and indicate that hcp nickel nanoparticles are more reactive to form Ni(OH)2 and lead to more electroactive Ni(OH)2 structure. The hcp nickel nanoparticles-modified electrode showed the best sensitivity (0.258 μA L μmol(-1)) and detection limit (2.4 μmol L(-1)) toward glycerol.

  13. Electrochemically prepared surface-enhanced Raman scattering-active silver substrates with improved stabilities

    NASA Astrophysics Data System (ADS)

    Yang, Kuang-Hsuan; Liu, Yu-Chuan; Yu, Chung-Chin; Chen, Bo-Chuen

    2011-01-01

    In this work, SiO 2 nanoparticles-modified surface-enhanced Raman scattering (SERS)-active silver substrates were prepared by electrochemical oxidation-reduction cycles (ORC) methods in 0.1 N HCl aqueous solutions containing 1 mM SiO 2 nanoparticles to improve their thermal stabilities and anti-aging abilities in SERS performances. Then these SERS-active substrates were further modified with different contents of SiO 2 nanoparticles to improve their corresponding SERS performances. Experimental results indicate that the operation temperature can be significantly raised from 125 to 175 °C based on this modified SERS-active Ag substrate. Also, the aging in SERS intensity is also depressed on this modified Ag substrate due to the contribution of SiO 2 nanoparticles. Moreover, the SERS enhancement capability on this modified Ag substrate is gradually raised from 25 °C to a maximum at 55 °C and monotonically decreased from 55 to 60 °C. This is a 10 °C delay as compared with the similar phenomenon observed on the unmodified Ag substrate.

  14. Electrochemical Evaluation of Pyrite Films Prepared by Plasma Spraying

    SciTech Connect

    Guidotti, R.A.; Reinhardt, F.W.

    1998-10-30

    Thermally activated batteries use electrodes that are typically fabricated by cold pressing of powder. In the LiSi/FeS2 system, natural (mineral) pyrite is used for the cathode. In an effort to increase the energy density and specific energy of these batteries, flame and plasma spraying to form thin films of pyrite cathodes were evaluated. The films were deposited on a 304 stainless steel substrate (current collector) and were characterized by scanning electron microscopy and x-ray dlfllaction. The films were electrochemically tested in single cells at 5000C and the petiormance compared to that of standard cells made with cold-pressed powders. The best results were obtained with material deposited by de-arc plasma spraying with a proprietq additive to suppress thermal decomposion of the pyrite.

  15. Green synthesis of manganese oxide nanoparticles for the electrochemical sensing of p-nitrophenol

    NASA Astrophysics Data System (ADS)

    Kumar, Vineet; Singh, Kulvinder; Panwar, Shaily; Mehta, Surinder Kumar

    2017-03-01

    Manganese oxide (MnO) NPs are widely used in contaminant sensing, drug delivery, data storage, catalysis and biomedical imaging. Green synthesis of NPs is important due to increased concern of environmental pollution. Green chemistry based synthesis of NPs is preferred due to its ecofriendly nature. In this study, MnO NPs of different sizes were synthesized in aqueous medium using clove, i.e., Syzygium aromaticum extract (CE) as reducing and stabilizing agents. These NPs were used for the electrochemical sensing of p-nitrophenol (PNP). The synthesis of MnO NPs was over in 30 min. MnO NPs of different sizes were obtained by varying metal ion concentration, metal ion volume ratio, CE concentration, CE volume ratio, and incubation temperature. Selectively, 4 nm MnO NPs were used for electrochemical sensing of paranitrophenol. The MnO NPs modified gold electrodes detected PNP with good sensitivity, 0.16 µA µM-1 cm2. The limit of PNP detection was 15.65 µM. The MnO NPs prepared using CE based green chemistry approach is useful for PNP sensing. These NPs can also be useful for various in vivo applications in which the NPs come in human contact.

  16. Direct and environmentally benign synthesis of manganese oxide/graphene composites from graphite for electrochemical capacitors

    NASA Astrophysics Data System (ADS)

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

    2015-05-01

    We develop a direct and environmentally benign method to prepare manganese oxide (Mn3O4)/graphene composites via one-step hydrothermal synthesis from graphite without using strong acids and toxic reducing agents. Structural and morphological analyses reveals that the irregularly shaped Mn3O4 nanoparticles are well-dispersed on the graphene flakes. Cyclic voltammetry and galvanostatic charge-discharge tests indicate that the charge-storing mechanism of the Mn3O4/graphene composites is pseudocapacitive. The Mn3O4/graphene composite exhibits a specific capacitance of 367 F/g at a current density of 5 A/g. After 3000 charge-discharge cycles, the Mn3O4/graphene electrode retains 91.8% of its initial specific capacitance. From electrochemical impedance spectra, it is evident that the changes in both the equivalent series resistance and charge-transfer resistance of the Mn3O4/graphene electrode before and after 3000 charge-discharge cycles are small, indicating good cycling and electrochemical stability of the Mn3O4/graphene electrode.

  17. A comparison study of macrocyclic hosts functionalized reduced graphene oxide for electrochemical recognition of tadalafil.

    PubMed

    Zhao, Hui; Yang, Long; Li, Yucong; Ran, Xin; Ye, Hanzhang; Zhao, Genfu; Zhang, Yanqiong; Liu, Feng; Li, Can-Peng

    2017-03-15

    The present work described the comparison of β-cyclodextrin (β-CD) and p-sulfonated calix[6]arene (SCX6) functionalized reduced graphene oxide (RGO) for recognition of tadalafil. In this study, tadalafil and two macrocycles (β-CD and SCX6) were selected as the guest and host molecules, respectively. The inclusion complexes of β-CD/tadalafil and SCX6/tadalafil were studied by UV spectroscopy and molecular simulation calculations, proving the higher supermolecular recognition capability of SCX6 than β-CD towards tadalafil. The β-CD@RGO and SCX6@RGO composites were prepared by a wet-chemical route. The obtained composites were characterized by Fourier transform infrared spectrometry, thermogravimetric analysis, atomic force microscopy, and zeta potential. The SCX6@RGO showed a higher electrochemical response than β-CD@RGO, which was caused by the higher recognition capability of SCX6 than β-CD. By combining the merits of SCX6 and the RGO, a sensitive electrochemical sensing platform was developed based on the SCX6@RGO nanohybrids. A linear response range of 0.1-50 μM and 50-1000 μM for tadalafil with a low detection limit of 0.045 μM (S/N=3) was obtained by using this method. The constructed sensing platform was successfully used to determine tadalafil in herbal sexual health products and spiked human serum samples, suggesting its promising analytical applications for the trace level determination of tadalafil.

  18. Enhancement of corrosion resistance of polypyrrole using metal oxide nanoparticles: Potentiodynamic and electrochemical impedance spectroscopy study.

    PubMed

    Hosseini, Marzieh; Fotouhi, Lida; Ehsani, Ali; Naseri, Maryam

    2017-11-01

    We introduce a simple and facile strategy for dispersing of nanoparticles within a p-type conducting polymer matrix by in situ electropolymerization using oxalic acid as the supporting electrolyte. Coatings prepared from polypyrrole-nano-metal oxide particles synthesized by in situ polymerization were found to exhibit excellent corrosion resistance much superior to polypyrrole (Ppy) in aggressive environments. The anti-corrosion behavior of polypyrrole films in different states and the presence of TiO2, Mn2O3 and ZnO nanoparticles synthesized by electropolymerization on Al electrodes have been investigated in corrosive solutions using potentiodynamic polarization and electrochemical impedance spectroscopy. The electrochemical response of the coated electrodes in polymer and nanocomposite state was compared with bare electrodes. The use of TiO2 nanoparticles has proved to be a great improvement in the performances of polypyrrole films for corrosion protection of Al samples. The polypyrrole synthesized in the presence of TiO2 nanoparticles coated electrodes offered a noticeable enhancement of protection against corrosion processes. The exceptional improvement of performance of these coatings has been associated with the increase in barrier to diffusion, prevention of charge transport by the nanosize TiO2, redox properties of polypyrrole as well as very large surface area available for the liberation of dopant due to nano-size additive. Copyright © 2017 Elsevier Inc. All rights reserved.

  19. Concurrent electropolymerization of aniline and electrochemical deposition of tungsten oxide for supercapacitor

    NASA Astrophysics Data System (ADS)

    Geng, Jin-Wang; Ye, Yin-Jian; Guo, Di; Liu, Xiao-Xia

    2017-02-01

    Polyaniline-tungsten oxide composite films (PANI-WOx) were prepared through concurrent electropolymerization of aniline and electrochemical deposition of tungsten oxide on partial exfoliated graphite (Ex-GF) for pseudocapacitive materials. The influence of aniline to WOx precursor ratio on pseudocapacitive properties of the afforded PANI-WOx/Ex-GF composite was investigated. PW-2:1/Ex-GF made from the solution containing aniline and WOx precursor in 2:1 ratio displayed a high specific capacitance (408 F g-1/408 mF cm-2 at 1 A g-1/1 mA cm-2) in a wide charge storage potential window of -0.6-0.7 V vs. SCE, leading to a high energy density of 95.8 Wh kg-1 at 650 W kg-1. Due to the synergistic effect between WOx and PANI, the composite showed much improved cyclic stability (91.6% capacitance retention after 5000 galvanostatic charge-discharge cycles) compared to similarly prepared PANI/Ex-GF (69.1% capacitance after 5000 charge-discharge cycles). The assembled symmetric model supercapacitor, by using PW-2:1/Ex-GF as both of the electrodes, also displayed good stability and high energy density, demonstrating that the PANI-WOx composite is promising electrode material for high-performance supercapacitor.

  20. Scalable Preparation of Ternary Hierarchical Silicon Oxide-Nickel-Graphite Composites for Lithium-Ion Batteries.

    PubMed

    Wang, Jing; Bao, Wurigumula; Ma, Lu; Tan, Guoqiang; Su, Yuefeng; Chen, Shi; Wu, Feng; Lu, Jun; Amine, Khalil

    2015-12-07

    Silicon monoxide is a promising anode candidate because of its high theoretical capacity and good cycle performance. To solve the problems associated with this material, including large volume changes during charge-discharge processes, we report a ternary hierarchical silicon oxide-nickel-graphite composite prepared by a facile two-step ball-milling method. The composite consists of nano-Si dispersed silicon oxides embedded in nano-Ni/graphite matrices (Si@SiOx /Ni/graphite). In the composite, crystalline nano-Si particles are generated by the mechanochemical reduction of SiO by ball milling with Ni. These nano-Si dispersed oxides have abundant electrochemical activity and can provide high Li-ion storage capacity. Furthermore, the milled nano-Ni/graphite matrices stick well to active materials and interconnect to form a crosslinked framework, which functions as an electrical highway and a mechanical backbone so that all silicon oxide particles become electrochemically active. Owing to these advanced structural and electrochemical characteristics, the composite enhances the utilization efficiency of SiO, accommodates its large volume expansion upon cycling, and has good ionic and electronic conductivity. The composite electrodes thus exhibit substantial improvements in electrochemical performance. This ternary hierarchical Si@SiOx /Ni/graphite composite is a promising candidate anode material for high-energy lithium-ion batteries. Additionally, the mechanochemical ball-milling method is low cost and easy to reproduce, indicating potential for the commercial production of the composite materials.

  1. Preparation of selective and sensitive electrochemically treated pencil graphite electrodes for the determination of uric acid in urine and blood serum.

    PubMed

    Ozcan, Ali; Sahin, Yücel

    2010-07-15

    In this study, the preparation of electrochemically treated pencil graphite (ETPG) electrodes in the mixture of lithium perchlorate and sodium carbonate solutions was investigated for the first time in the literature. The prepared ETPG electrodes showed high selectivity and sensitivity for uric acid (UA) oxidation over ascorbic acid and dopamine. Differential pulse voltammetry (DPV) was used as electrochemical method. The parameters affecting the UA oxidation were investigated. The optimal pH for UA oxidation was determined as 2. The adsorption of UA on ETPG surface reached saturation in 180s. The oxidation peak current values versus UA concentration at the ETPG electrode showed linearity in the range from 0.05 microM to 10.0 microM (R(2)=0.9962) with a detection limit of 1.5 nM (S/N=3). The oxidation peak of UA on the ETPG electrode did not show any significant change in the presence of certain interferents except bovine serum albumin. The prepared electrodes showed good fabrication reproducibility. The analytical applications of the prepared electrodes were tested by using human urine and blood serum samples. The recovery results of different amounts of UA in urine were varied between 98.6% and 106.4% implying no matrix effect. It was observed that the standard addition method was more satisfactory in the case of blood serum samples.

  2. Ultrafast electrochemical preparation of graphene/CoS nanosheet counter electrodes for efficient dye-sensitized solar cells

    SciTech Connect

    Zhu, Chongyang; Zhu, Yimei; Min, Huihua; Xu, Feng; Chen, Jing; Dong, Hui; Tong, Ling; Sun, Litao

    2015-10-05

    Utilizing inexpensive, high-efficiency counter electrodes (CEs) to replace the traditional platinum counterparts in dye-sensitized solar cells (DSSCs) is worthwhile. In this paper, we detail how we synchronously prepared composite CEs of CoS nanosheet arrays and reduced graphene oxide (rGO) layers for the first time via a low temperature, ultrafast one-step electrochemical strategy. With this approach, the whole fabrication process of the composite CEs was only a small percentage of the average time (~15 hours) using other methods. The DSSC assembled with the rGO–CoS composite CE achieved an enhanced power conversion efficiency (PCE) of 8.34%, which is dramatically higher than 6.27% of pure CoS CE-based DSSC and even exceeds 7.50% of Pt CE-based DSSC. The outstanding PCE breakthrough is undoubtedly attributed to the enhancement in electrocatalytic ability of the rGO–CoS composite CE due to the incorporation of highly conducting rGO layers and the GO layers-induced growth of CoS nanosheet arrays with higher density and larger surface area. Therefore, lower charge-transfer resistance and higher exchange current density can be achieved as corroborated by the electrochemical impedance spectra (EIS) and Tafel polarization curves (TPCs). As a result, further experiments also proved that the electrochemical strategy exhibited its universality of fabricating other graphene-enhanced chalcogenide functional composite films.

  3. Ultrafast electrochemical preparation of graphene/CoS nanosheet counter electrodes for efficient dye-sensitized solar cells

    DOE PAGES

    Zhu, Chongyang; Zhu, Yimei; Min, Huihua; ...

    2015-10-05

    Utilizing inexpensive, high-efficiency counter electrodes (CEs) to replace the traditional platinum counterparts in dye-sensitized solar cells (DSSCs) is worthwhile. In this paper, we detail how we synchronously prepared composite CEs of CoS nanosheet arrays and reduced graphene oxide (rGO) layers for the first time via a low temperature, ultrafast one-step electrochemical strategy. With this approach, the whole fabrication process of the composite CEs was only a small percentage of the average time (~15 hours) using other methods. The DSSC assembled with the rGO–CoS composite CE achieved an enhanced power conversion efficiency (PCE) of 8.34%, which is dramatically higher than 6.27%more » of pure CoS CE-based DSSC and even exceeds 7.50% of Pt CE-based DSSC. The outstanding PCE breakthrough is undoubtedly attributed to the enhancement in electrocatalytic ability of the rGO–CoS composite CE due to the incorporation of highly conducting rGO layers and the GO layers-induced growth of CoS nanosheet arrays with higher density and larger surface area. Therefore, lower charge-transfer resistance and higher exchange current density can be achieved as corroborated by the electrochemical impedance spectra (EIS) and Tafel polarization curves (TPCs). As a result, further experiments also proved that the electrochemical strategy exhibited its universality of fabricating other graphene-enhanced chalcogenide functional composite films.« less

  4. Electrochemical gas-electricity cogeneration through direct carbon solid oxide fuel cells

    NASA Astrophysics Data System (ADS)

    Xie, Yongmin; Cai, Weizi; Xiao, Jie; Tang, Yubao; Liu, Jiang; Liu, Meilin

    2015-03-01

    Solid oxide fuel cells (SOFCs), with yttrium stabilized zirconia (YSZ) as electrolyte, composite of strontium-doped lanthanum manganate (LSM) and YSZ as cathode, and cermet of silver and gadolinium-doped ceria (GDC) as anode, are prepared and tested with 5wt% Fe-loaded activated carbon as fuel and ambient air as oxidant. It is found that electricity and CO gas can be cogenerated in the direct carbon SOFCs through the electrochemical oxidation of CO and the Boudouard reaction. The gas-electricity cogeneration performances are investigated by taking the operating time of the DC-SOFCs as a measure of rate decrease of the Boudouard reaction. Three single cells and a two-cell-stack are tested and characterized in terms of electrical power output, CO production rate, electrical conversion efficiency, and overall conversion efficiency. It turns out that a rapid rate of the Boudouard reaction is necessary for getting high electrical power and CO production. Taking the emitted CO as part of the power output, an overall efficiency of 76.5% for the single cell, and of 72.5% for the stack, is obtained.

  5. An electrochemical dopamine aptasensor incorporating silver nanoparticle, functionalized carbon nanotubes and graphene oxide for signal amplification.

    PubMed

    Bahrami, Shokoh; Abbasi, Amir Reza; Roushani, Mahmoud; Derikvand, Zohreh; Azadbakht, Azadeh

    2016-10-01

    In this work, immobilization of a dopamine (DA) aptamer was performed at the surface of an amino functionalized silver nanoparticle-carbon nanotube graphene oxide (AgNPs/CNTs/GO) nanocomposite. A 58-mer DA-aptamer was immobilized through the formation of phosphoramidate bonds between the amino group of chitosan and the phosphate group of the aptamer at the 5' end. An AgNPs/CNTs/GO nanocomposite was employed as a highly catalytic label for electrochemical detection of DA based on electrocatalytic activity of the nanocomposite toward hydrogen peroxide (H2O2). Interaction of DA with the aptamer caused conformational changes of the aptamer which, in turn, decreased H2O2 oxidation and reduction peak currents. On the other hand, the presumed folding of the DA-aptamer complexes on the sensing interface inhibited the electrocatalytic activity of AgNPs/CNTs/GO toward H2O2. Sensitive quantitative detection of DA was carried out by monitoring the decrease of differential pulse voltammetric (DPV) responses of AgNPs/CNTs/GO nanocomposite toward H2O2 oxidation. The DPV signal linearly decreased with increased concentration of DA from 3 to 110nmolL(-1) with a detection limit of 700±19.23pmolL(-1). Simple preparation, low operation cost, speed and validity are the decisive factors of this method motivating its application to biosensing investigation.

  6. Electrochemical synthesis of new magnetic mixed oxides of Sr and Fe: Composition, magnetic properties, and microstructure

    SciTech Connect

    Amigo, R.; Asenjo, J.; Krotenko, E.; Torres, F.; Tejada, J.; Brillas, E.

    2000-02-01

    An electrochemical method for the preparation of magnetic nanoparticles of new Sr-Fe oxides is presented in this work. It consists of the electrolysis of nitrate or chloride solutions with Sr{sup 2+} and Fe{sup 3+} salts using commercial Fe electrodes. Magnetic materials are collected as precipitates from nitrate media in the pH range 1-3 and from chloride media within the pH range 1--12. The presence of 100--300 ppm aniline in acidic nitrate media yields a decrease in energy cost and particle size. Inductively coupled plasma analysis of materials and energy-dispersive X-ray spectrometry of single particles confirm that they are composed of mixed oxides of Sr and Fe. All synthesized materials crystallize as inverse cubic spinels, usually with intermediate structures between magnetite and maghemite. They are formed by nanoparticles with average sizes from 2 nm to {approximately} 50 nm, as observed by scanning electron microscopy. The electrogenerated mixed oxides have higher saturation magnetization, but lower remanent magnetization and coercive field, than commercial strontium hexaferrite with micrometric particle size.

  7. Electrochemical Stripping of Atomic Oxygen on Single-Crystalline Platinum: Bridging Gas-Phase and Electrochemical Oxidation

    PubMed Central

    2017-01-01

    To understand the interaction between Pt and surface oxygenated species in electrocatalysis, this paper correlates the electrochemistry of atomic oxygen on Pt formed in the gas phase with electrochemically generated oxygen species on a variety of single-crystal platinum surfaces. The atomic oxygen adsorbed on single-crystalline Pt electrodes, made by thermal dissociation of molecular oxygen, is used for voltammetry measurements in acidic electrolytes (HClO4 and H2SO4). The essential knowledge of coverage, binding energy, and surface construction of atomic oxygen is correlated with the charge, potential, and shape of voltammograms, respectively. The differences of the voltammograms between the oxide made by thermal dissociation of molecular oxygen and electrochemical oxidation imply that atomic oxygen is not an intermediate of the electrochemical oxidation of Pt(111). The reconstruction of (100) terrace and step and the low-potential stripping of atomic oxygen on (111) step site provide insight into the first stages of degradation of Pt-based electrocatalysts. PMID:28225278

  8. Improvement of electron emission characteristics of porous silicon emitter by using cathode reduction and electrochemical oxidation

    NASA Astrophysics Data System (ADS)

    Li, He; Wenjiang, Wang; Xiaoning, Zhang

    2017-03-01

    A new simple and convenient post-treat technique combined the cathode reduction (CR) and electrochemical oxidation (ECO) was proposed to improve the electron emission properties of the surface-emitting cold cathodes based on the porous silicon (PS). It is demonstrated here that by introducing this new technique combined CR and ECO, the emission properties of the diode have been significantly improved than those as-prepared samples. The experimental results showed that the emission current densities and efficiencies of sample treated by CR were 62 μA/cm2 and 12.10‰, respectively, nearly 2 orders of magnitude higher than those of as-prepared sample. Furthermore, the CR-treated PS emitter shows higher repeatability and stability compared with the as-prepared PS emitter. The scanning electron microscope (SEM), atomic force microscope (AFM), energy dispersive spectrometer (EDS), furier transformed infrared (FTIR) spectroscopy results indicated that the improved mechanism is mainly due to the passivation of the PS, which not only improve the PS morphology by the passivation of the H+ but also improve the uniformity of the oxygen content distribution in the whole PS layer. Therefore, the method combined the CR treatment and ECO is expected to be a valuable technique to enhance the electron emission characteristics of the PS emitter.

  9. Preparation of a manganese titanate nanosensor: Application in electrochemical studies of captopril in the presence of para-aminobenzoic acid.

    PubMed

    Ghoreishi, Sayed Mehdi; Karamali, Elham; Khoobi, Asma; Enhessari, Morteza

    2015-10-15

    This study reports the synthesis and characterization of a novel nanostructure-based electrode for electrochemical studies and determination of captopril (CP). At first manganese titanate nanoceramics were synthesized by the sol-gel method. The structural evaluations of the pure nanopowders were investigated by different techniques such as X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Then it was used to prepare a new nanostructured manganese titanate carbon paste electrode (MnTiO3/CPE). The characterization of the modified sensor was carried out by comprehensive techniques such as electrochemical impedance spectroscopy (EIS), SEM, and voltammetry. Subsequently, the modified electrode was used for CP catalytic oxidation in the presence of para-aminobenzoic acid (PABA) as a mediator. The results showed that PABA has high catalytic activity for CP oxidation. The electrochemical behavior of CP was studied by cyclic voltammetry (CV), linear sweep voltammetry (LSV), chronoamperometry (CHA), and differential pulse voltammetry (DPV) techniques. Under the optimized conditions, the catalytic oxidation peak current of CP showed two linear dynamic concentration ranges of 1.0 × 10(-8) to 1.0 × 10(-7) and 1.0 × 10(-7) to 1.0 × 10(-6), with a detection limit of 1.6 nM (signal/noise = 3), using the DPV technique. Finally, the proposed method was successfully applied for determination of CP in pharmaceutical and biological samples. Copyright © 2015 Elsevier Inc. All rights reserved.

  10. Validation of electrochemical determination of zinc in selected pharmaceutical preparations.

    PubMed

    Lutka, Anna; Kokot, Zenon; Powidzka, Hanna

    2004-01-01

    A procedure of voltammetric (DP) determination of zinc in two selected pharmaceutical preparations was validated. The source of zinc in the first of them (Bio-Cynk) was the organic salt-gluconate, while the second (Zincteral) contained zinc sulfate. In order to transform zinc into solution, the samples of powdered tablets of each preparation underwent the extraction or mineralisation procedure. The concentration of zinc in solution was determined by differential pulse voltammetry (DP). In the validation process, the selectivity, accuracy, precision and linearity of DP determination of zinc in both preparations were examined. Zinc was determined within the concentration range of 1-20 ppm: the mean recoveries approached 98% in the case of Bio-Cynk and 100% for Zincteral; the errors of determination (RDS) were 2.98-11.5% for Bio-Cynk and 3.06-5.32% for Zincteral, respectively.

  11. Preparation of Electrochemical Biosensor for Detection of Organophosphorus Pesticides

    PubMed Central

    Gothwal, Ashish; Beniwal, Puneet; Dhull, Vikas

    2014-01-01

    Polyvinyl chloride (PVC) can be used to develop reaction beaker which acts as electrochemical cell for the measurement of OP pesticides. Being chemically inert, corrosion resistant, and easy in molding to various shapes and size, PVC can be used for the immobilization of enzyme. Organophosphorus hydrolase was immobilized covalently onto the chemically activated inner surface of PVC beaker by using glutaraldehyde as a coupling agent. The carbon nanotubes paste working electrode was constructed for amperometric measurement at a potential of +0.8 V. The biosensor showed optimum response at pH 8.0 with incubation temperature of 40°C. K m and I max for substrate (methyl parathion) were 322.58 µM and 1.1 µA, respectively. Evaluation study showed a correlation of 0.985, which was in agreement with the standard method. The OPH biosensor lost 50% of its initial activity after its regular use for 25 times over a period of 50 days when stored in 0.1 M sodium phosphate buffer, pH 8.0 at 4°C. No interference was observed by interfering species. PMID:25667593

  12. Preparation and electrochemical performance of ultra-short carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Wang, Xiao X.; Wang, Jian N.; Su, Lian F.

    Current carbon nanotubes (CNTs) are typically synthesized with micrometer lengths, low dispersion and low purity and thus oppose their applications in many fields. In this study, we make the first report on using a Fe compound (FeS) as a catalyst for controlling the length of CNTs to be less than 300 nm. This is achieved by dissolution of a proper proportion of ferrocene and thiophene in alcohol and pyrolysis of this solution at high temperature. Sulfur, resulting from the decomposition of thiophene, is shown to play key roles in promoting the growth of CNTs and limiting their length. The reason is suggested to be that FeS retards the dissociation of carbon source and diffusion of carbon in it as compared with pure Fe. Short CNTs from the present direct synthesis and from our previous solid-state cutting are used as an electrode material in Li-ion batteries and catalyst supports in fuel cells. Compared with conventional long CNTs, short CNTs show much better electrochemical performance. Due to the simplicity of the present synthetic technique, it may be used for mass production of short CNTs. Furthermore, the application of such a new material may be investigated in wide areas such as information technology, biomedicine, environmental and energy industries.

  13. Optimal preparation of the ECC ozonesonde. [electrochemical cells

    NASA Technical Reports Server (NTRS)

    Thornton, D. C.

    1982-01-01

    The ECC background current was identified as the removal of residual tri-iodide (iodine) as the cell approaches equilibrium. The altitude dependence of this source of the background current is expected to be only slowly changed in the troposphere with a more rapid decrease in the stratosphere. Oxygen does not play a role in the background current except in the unlikely situation where the electrodes have had all forms of iodine removed from them and the electrodes have not re-equilibrated with the sonde solutions before use. A solution mass transport parameter in the ECC was identified and its altitude dependence determined. The mass transport of tri-iodide dominates in the chemical transduction of ozone to electrical signal. The effect of the mass transport on the ECC background current is predicted. An electrochemical model of the ECC has been developed to predict the response of the ECC to various ozone vertical profiles. The model corresponds very closely to the performance of the ECC in the laboratory. Based on this model, an ECC with no background current is predicted to give total ozone values within 1% of the correct value, although the vertical profile may be in error by as much as + or - 15%.

  14. Study of electrochemically prepared CuInSe2 thin films

    NASA Astrophysics Data System (ADS)

    Dhanwate, Vishakha N.; Chaure, N. B.

    2012-06-01

    We report the deposition of Copper Indium diselenide (CIS) films were prepared by electrochemical deposition technique, onto FTO coating glass substrates. The deposition potential was optimized with the aid of cyclic voltammetry (CV) experiments. The deposition conditions (pH, bath temperature, stirring etc.) and chemical concentration of ionic species were optimized. CIS layers were deposited at different potentials close to the plateau observed by CV at 40 0C using a three-electrode conventional electrochemical cell. The layers were characterized thoroughly to understand the structure, composition and surface morphology.

  15. STEP wastewater treatment: a solar thermal electrochemical process for pollutant oxidation.

    PubMed

    Wang, Baohui; Wu, Hongjun; Zhang, Guoxue; Licht, Stuart

    2012-10-01

    A solar thermal electrochemical production (STEP) pathway was established to utilize solar energy to drive useful chemical processes. In this paper, we use experimental chemistry for efficient STEP wastewater treatment, and suggest a theory based on the decreasing stability of organic pollutants (hydrocarbon oxidation potentials) with increasing temperature. Exemplified by the solar thermal electrochemical oxidation of phenol, the fundamental model and experimental system components of this process outline a general method for the oxidation of environmentally stable organic pollutants into carbon dioxide, which is easily removed. Using thermodynamic calculations we show a sharply decreasing phenol oxidation potential with increasing temperature. The experimental results demonstrate that this increased temperature can be supplied by solar thermal heating. In combination this drives electrochemical phenol removal with enhanced oxidation efficiency through (i) a thermodynamically driven decrease in the energy needed to fuel the process and (ii) improved kinetics to sustain high rates of phenol oxidation at low electrochemical overpotential. The STEP wastewater treatment process is synergistic in that it is performed with higher efficiency than either electrochemical or photovoltaic conversion process acting alone. STEP is a green, efficient, safe, and sustainable process for organic wastewater treatment driven solely by solar energy.

  16. Preparation of Ferrotitanium Alloy from Ilmenite by Electrochemical Reduction in Chloride Molten Salts

    NASA Astrophysics Data System (ADS)

    Qi, Can-can; Hua, Yi-xin; Chen, Kong-hao; Jie, Ya-fei; Zhou, Zhong-ren; Ru, Juan-jian; Xiong, Li; Gong, Kai

    2016-02-01

    Ferrotitanium alloy is prepared by electrochemical reduction from ilmenite in LiCl-KCl and LiCl-KCl-CaCl2 molten salts, respectively. The products prepared are observed by x-ray diffraction (XRD). It is shown that Fe2Ti can be prepared from ilmenite in LiCl-KCl molten salt at 1073 K with a cell voltage of 3.2 V. Ilmenite can be electrochemically reduced to FeTi in LiCl-KCl-CaCl2 molten salt under the same condition. It is indicated that CaCl2 can promote the reaction and is favors the deoxidization of the FeTiO3.

  17. Design of a new nanocomposite between bismuth nanoparticles and graphene oxide for development of electrochemical sensors.

    PubMed

    Bindewald, Eduardo H; Schibelbain, Arthur F; Papi, Maurício A P; Neiva, Eduardo G C; Zarbin, Aldo J G; Bergamini, Márcio F; Marcolino-Júnior, Luiz H

    2017-10-01

    This study describes a new route for preparation of a nanocomposite between graphene oxide (GO) and bismuth nanoparticles (BiNPs) and its evaluation as modifier electrode for development of electrochemical sensors. BiNPs were synthesized under ultrasound conditions using Bi(NO3)3 as metal precursor and ascorbic acid (AA) as reducing agent/passivating. Some experimental parameters of BiNPs synthesis such as Bi(3+):AA molar ratio and reaction time were conducted aiming the best voltammetric performance of the sensor. Glassy carbon electrodes (GCE) were modified by drop-casting with the BiNPs dispersions and anodic stripping voltammetry measurements were performed and revealed an improvement in the sensitivityfor determination of Cd(II) and Pb(II) compared to an unmodified electrode. The best electrochemical response was obtained for a BiNPs synthesis with Bi(3+):AA molar ratio of 1:6 and reaction time of 10min, which yielded Bi metallic nanoparticles with average size of 5.4nm confirmed by XRD and TEM images, respectively. GO was produced by graphite oxidation using potassium permanganate and exfoliated with an ultrasound tip. GO-BiNPs nanocomposite was obtained by a simple mixture of GO and BiNPs dispersions in water and kept under ultrasonic bath for 1h. GCE were modified with a nanocomposite suspension containing 0.3 and 1.5mgmL(-1) of GO and BiNPs in water, respectively. Under optimized conditions, the proposed nanocomposite was evaluated on the voltammetric determination of Pb (II) and Cd (II), leading to a linear response range between 0.1 and 1.4μmolL(-1) for both cations, with limit of detection of 30 and 27nmolL(-1), respectively. These results indicate the great potential of the GO-BiNPs nanocomposite for improving the sensitivity of voltammetric procedures. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Mediated electrochemical oxidation as an alternative to incineration for mixed wastes

    SciTech Connect

    Chiba, Z.; Schumacher, B.; Lewis, P.; Murguia, L.

    1995-02-01

    Mediated Electrochemical Oxidation (MEO) is an aqueous process which oxidizes organics electrochemically at low temperatures and ambient pressures. The process can be used to treat mixed wastes containing hazardous organics by destroying the organic components of the wastes. The radioactive components of the wastes are dissolved in the electrolyte where they can be recovered if desired, or immobilized for disposal. The process of destroying organics is accomplished via a mediator, which is in the form of metallic ions in solution. At Lawrence Livermore National Laboratory (LLNL) we have worked with worked with several mediators, including silver, cobalt and cerium. We have tested mediators in nitric as well as sulfuric acids. We have recently completed extensive experimental studies on cobalt-sulfuric acid and silver-nitric acid systems for destroying the major organic components of Rocky Flats Plant combustible mixed wastes. Organics tested were: Trimsol (a cutting oil), cellulose (including paper and cloth), rubber (latex), plastics (Tyvek, polyethylene and polyvinyl chloride) and biomass (bacteria). The process was capable of destroying almost all of the organics tested, attaining high destruction efficiencies at reasonable coulombic efficiencies. The only exception was polyvinyl chloride, which was destroyed very slowly resulting in poor coulombic efficiencies. Besides the process development work mentioned above, we are working on the design of a pilot-plant scale integrated system to be installed in the Mixed Waste Management Facility (MWMF) at LLNL. The system will also be completely integrated with upstream and downstream processes (for example, feed preparation, off-gas and water treatment, and final forms encapsulation). The conceptual design for the NEO-MWMF system has been completed and preliminary design work has been initiated. Demonstration of the process with low-level mixed wastes is expected to commence in 1998.

  19. Nanoporous ZnO prepared by electrochemical anodization deposition

    NASA Astrophysics Data System (ADS)

    Chuah, L. S.; Hassan, Z.; Mohd Bakhori, S. K.

    2012-04-01

    Anodic physical deposition is a method that joins technical simplicity, environment friendly, non-toxic, low investment cost, and ease in morphology control. Nanoporous ZnO with high internal rough surface and polycrystalline nature has been prepared via a simple chemical technique. Anodization of Znic (Zn) foil was studied in a mixed of ammonium sulfate and sodium hydroxide solution under the affect of various anodization durations. The as-prepared samples were studied by X-ray diffraction (XRD), and energy dispersive analysis of X-rays (EDX). An optical characterization by a Raman spectrometer was performed to investigate their optical properties. The PL and Raman results revealed both good compromise with the features of our samples and dormant for forthcoming utilizations for example smart sensors system and other modern solid state technologies. The formation of porous structures has been confirmed by Raman spectroscopy and scanning electron microscopy investigations.

  20. Nanoporous ZnO prepared by electrochemical anodization deposition

    NASA Astrophysics Data System (ADS)

    Chuah, L. S.; Hassan, Z.; Mohd Bakhori, S. K.

    2011-11-01

    Anodic physical deposition is a method that joins technical simplicity, environment friendly, non-toxic, low investment cost, and ease in morphology control. Nanoporous ZnO with high internal rough surface and polycrystalline nature has been prepared via a simple chemical technique. Anodization of Znic (Zn) foil was studied in a mixed of ammonium sulfate and sodium hydroxide solution under the affect of various anodization durations. The as-prepared samples were studied by X-ray diffraction (XRD), and energy dispersive analysis of X-rays (EDX). An optical characterization by a Raman spectrometer was performed to investigate their optical properties. The PL and Raman results revealed both good compromise with the features of our samples and dormant for forthcoming utilizations for example smart sensors system and other modern solid state technologies. The formation of porous structures has been confirmed by Raman spectroscopy and scanning electron microscopy investigations.

  1. Electrochemical oxidation of fluoroquinolone antibiotics: Mechanism, residual antibacterial activity and toxicity change.

    PubMed

    Zhu, Linyan; Santiago-Schübel, Beatrix; Xiao, Hongxia; Hollert, Henner; Kueppers, Stephan

    2016-10-01

    In this paper, we studied the electrochemical oxidation mechanisms of three typical fluoroquinolone antibiotics (FQs), and investigated residual antibacterial activity and toxicity changes after oxidation processes. Electrochemistry coupled to mass spectrometry (EC-MS) was used to study the oxidation processes of ciprofloxacin (CIP), norfloxacin (NOR) and ofloxacin (OFL). Eight oxidation products for each parent compound were identified and their chemical structures were elucidated. The transformation trend of each product, with the continuous increase of voltage from 0 to 3000 mV, was recorded by online EC-MS. The oxidation pathways were proposed based on the structural information and transformation trends of oxidation products. We found the oxidation mechanisms of FQs consisted of the hydroxylation and cleavage of piperazinyl ring via reactions with hydroxyl radicals, while the fluoroquinolone core remained intact. The antibacterial activity of the parent compounds and their oxidation mixtures was estimated using zone inhibition tests for gram-negative bacteria Salmonella typhimurium. It was found that the oxidation mixtures of CIP and NOR retained the antibacterial properties with lower activity compared to their parent compounds, while the antibacterial activity of OFL was almost eliminated after oxidation. Furthermore, the toxicity of the three FQs and their oxidation mixtures were evaluated using algal growth inhibition test (Desmodesmus subspicatus). The median effective concentration (EC50) values for the algal inhibition tests were calculated for the end point of growth rate. The toxicity of CIP and NOR to green algae after electrochemical oxidation, remained unchanged, while that of OFL significantly increased. The results presented in this paper contribute to an understanding of the electrochemical oxidation mechanisms of FQs, and highlight the potential environmental risks of FQs after electrochemical oxidation processes. Copyright © 2016 Elsevier

  2. Electrochemically assisted photocatalysis: Highly efficient treatment using thermal titanium oxides doped and non-doped electrodes for water disinfection.

    PubMed

    Dos Santos, Andreia Betina Kreuser; Claro, Elis Marina Turini; Montagnolli, Renato Nallin; Cruz, Jaqueline Matos; Lopes, Paulo Renato Matos; Bidoia, Ederio Dino

    2017-09-07

    Electrochemically assisted photocatalysis (by electronic drainage) is a highly promising method for disinfection of water. In this research, the efficiency of photolytic oxidation using UV-A radiation and electrochemically assisted photocatalysis (with electric potential of 1.5 V) was studied by using electrodes prepared by thermal treatment and doped with silver, for inactivation of Escherichia coli and Staphylococcus aureus. The Chick-Watson microorganism inactivation model was applied and the electrical energy consumption of the process was calculated. It was observed no significant inactivation of microorganisms when UV-A light or electric potential were applied separately. However, the electrochemically assisted photocatalytic process, with Ag-doped electrode completely inactivated the microbial population after 10 (E. coli) and 60 min (S. aureus). The best performing non-doped electrodes achieved 52.74% (E. coli) and 44.09% (S. aureus) inactivation rates after 60 min. Thus, electrochemically assisted photocatalytic activity was not only effective for the inactivation of microorganisms, but also notably low on electrical energy consumption during the treatment due to small current and low electric potential applied. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Pencil graphite electrodes for improved electrochemical detection of oleuropein by the combination of Natural Deep Eutectic Solvents and graphene oxide.

    PubMed

    Gomez, Federico J V; Spisso, Adrian; Silva, María Fernanda

    2017-09-07

    A novel methodology is presented for the enhanced electrochemical detection of oleuropein in complex plant matrices by Graphene Oxide Pencil Grahite Electrode (GOPGE) in combination with a buffer modified with a Natural Deep Eutectic Solvent, containing 10% (v/v) of Lactic acid, Glucose and H2 O (LGH). The electrochemical behavior of oleuropein in the modified-working buffer was examined using differential pulse voltammetry. The combination of both modifications, NADES modified buffer and nanomaterial modified electrode, LGH-GOPGE, resulted on a signal enhancement of 5.3 times higher than the bare electrode with unmodified buffer. A calibration curve of oleuropein was performed between 0.10 to 37 μM and a good linearity was obtained with a correlation coefficient of 0.989. Detection and quantification limits of the method were obtained as 30 and 102 nM, respectively. In addition, precision studies indicated that the voltammetric method was sufficiently repeatable, %RSD 0.01 and 3.16 (n = 5) for potential and intensity, respectively. Finally, the proposed electrochemical sensor was successfully applied to the determination of oleuropein in an olive leaf extract prepared by ultrasound-assisted extraction. The results obtained with the proposed electrochemical sensor were compared with Capillary Zone Electrophoresis analysis with satisfactory results. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  4. High Surface Area Antimony-Doped Tin Oxide Electrodes Templated by Graft Copolymerization. Applications in Electrochemical and Photoelectrochemical Catalysis

    SciTech Connect

    Luo, Hanlin; Fang, Zhen; Song, Na; Garvey, Timothy; Lopez, Rene; Meyer, Thomas J.

    2015-11-18

    Mesoporous ATO nanocrystalline electrodes of micrometer thicknesses have been prepared from ATO nanocrystals and the grafted copolymer templating agents poly vinyl chloride-g-poly(oxyethylene methacrylate). As-obtained electrodes have high interfacial surface areas, large pore volumes, and rapid intraoxide electron transfer. The resulting high surface area materials are useful substrates for electrochemically catalyzed water oxidation. With thin added shells of TiO2 deposited by atomic layer deposition (ALD) and a surface-bound Ru(II) polypyridyl chromophore, they become photoanodes for hydrogen generation in the presence of a reductive scavenger.

  5. Electrochemical Oxidative Decarboxylation of Malonic Acid Derivatives: A Method for the Synthesis of Ketals and Ketones.

    PubMed

    Ma, Xiaofeng; Luo, Xiya; Dochain, Simon; Mathot, Charlotte; Markò, István E

    2015-10-02

    A novel electrochemical oxidative decarboxylation of disubstituted malonic acids leading to dimethoxy ketals is described. In the presence of NH3, a wide range of disubstituted malonic acids was transformed into the corresponding ketals in good to excellent yields under electrochemical conditions. When the crude reaction mixture, obtained after electrolysis, was directly treated with 1 M aq HCl, the initially generated ketals were smoothly transformed into the corresponding ketones in a single vessel operation.

  6. Preparation of superhydrophobic silicon oxide nanowire surfaces.

    PubMed

    Coffinier, Yannick; Janel, Sébastien; Addad, Ahmed; Blossey, Ralf; Gengembre, Léon; Payen, Edmond; Boukherroub, Rabah

    2007-02-13

    The paper reports on the preparation of superhydrophobic amorphous silicon oxide nanowires (a-SiONWs) on silicon substrates with a contact angle greater than 150 degrees by means of surface roughness and self-assembly. Nanowires with an average mean diameter in the range 20-150 nm and 15-20 microm in length were obtained by the so-called solid-liquid-solid (SLS) technique. The porous nature and the high roughness of the resulting surfaces were confirmed by AFM imaging. The superhydrophobicity resulted from the combined effects of surface roughness and chemical modification with fluorodecyl trichlorosilane.

  7. Route of electrochemical oxidation of the antibiotic sulfamethoxazole on a mixed oxide anode.

    PubMed

    Hussain, Sajjad; Gul, Saima; Steter, Juliana R; Miwa, Douglas W; Motheo, Artur J

    2015-10-01

    The appearance of pharmaceutical compounds and their bioactive transformation products in aquatic environments is becoming an issue of increasing concern. In this study, the electrochemical oxidation of the widely used antibiotic sulfamethoxazole (SMX) was investigated using a commercial mixed oxide anode (Ti/Ru0.3Ti0.7O2) and a single compartment filter press-type flow reactor. The kinetics of SMX degradation was determined as a function of electrolyte composition, applied current density, and initial pH. Almost complete (98 %) degradation of SMX could be achieved within 30 min of electrolysis in 0.1 mol L(-1) NaCl solution at pH 3 with applied current densities ≥20 mA cm(-2). Nine major intermediates of the reaction were identified by LC-ESI-Q-TOF-MS (e.g., C6H9NO2S (m/z = 179), C6H4NOCl (m/z = 141), and C6H6O2 (m/z = 110)). The degradation followed various routes involving cleavage of the oxazole and benzene rings by hydroxyl and/or chlorine radicals, processes that could occur before or after rupture of the N-S bond, followed by oxidation of the remaining moieties. Analysis of the total organic carbon content revealed that the antibiotic was partially mineralized under the conditions employed and some inorganic ions, including NO3 (-) and SO4 (2-), could be identified. The results presented herein demonstrate the efficacy of the electrochemical process using a Ti/Ru0.3Ti0.7O2 anode for the remediation of wastewater containing the antibiotic SMX.

  8. Next-Generation Electrochemical Energy Materials for Intermediate Temperature Molten Oxide Fuel Cells and Ion Transport Molten Oxide Membranes.

    PubMed

    Belousov, Valery V

    2017-02-21

    High temperature electrochemical devices such as solid oxide fuel cells (SOFCs) and oxygen separators based on ceramic materials are used for efficient energy conversion. These devices generally operate in the temperature range of 800-1000 °C. The high operating temperatures lead to accelerated degradation of the SOFC and oxygen separator materials. To solve this problem, the operating temperatures of these electrochemical devices must be lowered. However, lowering the temperature is accompanied by decreasing the ionic conductivity of fuel cell electrolyte and oxygen separator membrane. Therefore, there is a need to search for alternative electrolyte and membrane materials that have high ionic conductivity at lower temperatures. A great many opportunities exist for molten oxides as electrochemical energy materials. Because of their unique electrochemical properties, the molten oxide innovations can offer significant benefits for improving energy efficiency. In particular, the newly developed electrochemical molten oxide materials show high ionic conductivities at intermediate temperatures (600-800 °C) and could be used in molten oxide fuel cells (MOFCs) and molten oxide membranes (MOMs). The molten oxide materials containing both solid grains and liquid channels at the grain boundaries have advantages compared to the ceramic materials. For example, the molten oxide materials are ductile, which solves a problem of thermal incompatibility (difference in coefficient of thermal expansion, CTE). Besides, the outstanding oxygen selectivity of MOM materials allows us to separate ultrahigh purity oxygen from air. For their part, the MOFC electrolytes show the highest ionic conductivity at intermediate temperatures. To evaluate the potential of molten oxide materials for technological applications, the relationship between the microstructure of these materials and their transport and mechanical properties must be revealed. This Account summarizes the latest results on

  9. Capsid protein oxidation in feline calicivirus using an electrochemical inactivation treatment.

    PubMed

    Shionoiri, Nozomi; Nogariya, Osamu; Tanaka, Masayoshi; Matsunaga, Tadashi; Tanaka, Tsuyoshi

    2015-01-01

    Pathogenic viral infections are an international public health concern, and viral disinfection has received increasing attention. Electrochemical treatment has been used for treatment of water contaminated by bacteria for several decades, and although in recent years several reports have investigated viral inactivation kinetics, the mode of action of viral inactivation by electrochemical treatment remains unclear. Here, we demonstrated the inactivation of feline calicivirus (FCV), a surrogate for human noroviruses, by electrochemical treatment in a developed flow-cell equipped with a screen-printed electrode. The viral infectivity titer was reduced by over 5 orders of magnitude after 15 min of treatment at 0.9V vs. Ag/AgCl. Proteomic study of electrochemically inactivated virus revealed oxidation of peptides located in the viral particles; oxidation was not observed in the non-treated sample. Furthermore, transmission electron microscopy revealed that viral particles in the treated sample had irregular structures. These results suggest that electrochemical treatment inactivates FCV via oxidation of peptides in the structural region, causing structural deformation of virus particles. This first report of viral protein damage through electrochemical treatment will contribute to broadening the understanding of viral inactivation mechanisms. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    NASA Astrophysics Data System (ADS)

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

    2016-02-01

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

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

    PubMed Central

    Chong, Soon Weng; Lai, Chin Wei; Abd Hamid, Sharifah Bee

    2016-01-01

    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. PMID:28787869

  12. Characterization and electrochemical application of carbon materials based on poly(phenylene oxide)

    NASA Astrophysics Data System (ADS)

    Gray, Hunter

    Carbon materials possess excellent electrical and surface properties for the next generation of energy storage devices. Polymers provide a carbon rich and tailorable precursor for the production of carbon materials. Therefore, activated carbons were prepared from poly(2,6-dimethyl-1,4-phenylene oxide) (PPO) via a three step process: thermal oxidation, carbonization, and activation with KOH. The activated carbons are predominately microporous with BET specific surface areas up to 2638 m2/g. Impedance spectroscopy revealed these carbons possess electrical conductivities comparable to commercial carbon blacks and consequently were employed in thin-film composite electrodes in electrochemical double-layer capacitors. Cyclic voltammetry confirmed maximum specific capacitances of 13.23 F/g and 2.848 F/g for aqueous and organic electrolyte systems, respectively. Additionally, carbon nanotubes were synthesized from PPO and other polymers with a nickel catalyst via chemical vapor deposition as revealed by transmission electron microscopy. This is the first report of carbon nanotubes produced from PPO.

  13. Preparation of electrochemically treated nanoporous pencil-graphite electrodes for the simultaneous determination of Pb and Cd in water samples.

    PubMed

    Dönmez, Koray B; Çetinkaya, Ebru; Deveci, Seda; Karadağ, Sevinç; Şahin, Yücel; Doğu, Mustafa

    2017-08-01

    A simple and rapid analytical method of determining Pb(2+) and Cd(2+) in water samples using an electrochemically pretreated pencil-graphite electrode (EP-PGE) is proposed for the first time in the literature. An electrochemically pretreated pencil-graphite electrode was prepared by performing potential cycling between -0.3 V and 2.0 V in 0.1 mol L(-1) H3PO4 solution to improve its ability to electrochemically sense Pb(2+) and Cd(2+) ions. Square-wave anodic stripping voltammetry (SWASV) was used as the electroanalytical method. The electroanalytical parameters that influence the stripping determination of Pb(2+) and Cd(2+) were optimized based on experimental results. The magnitude of the peak oxidation current was adjusted in order to optimize the value of each parameter. Applying the resulting disposable electrode under the optimized conditions led to good selectivity and sensitivity in the determination of Pb(2+) and Cd(2+) ions. Interference from coexisting ions was also investigated. The resulting sensor was successfully tested by applying it to a standard reference water sample. Under the optimized conditions, the limits of detection were 0.46 μg L(-1) for Pb(2+) and 1.11 μg L(-1) for Cd(2+) using the electrode. Relative standard deviations (%RSD) were 2.76 for Pb(2+) and 2.85 for Cd(2+). The linear working ranges of the electrode for Pb(2+) and Cd(2+) ion detection were 5-45 μg L(-1) and 10-40 μg L(-1), respectively. Graphical abstract Preparation of nanoporous pencil-graphite electrode by cyclic voltammetry and stripping voltammetric screening of Pb and Cd.

  14. Synthesis of Pb nanowires-Au nanoparticles nanostructure decorated with reduced graphene oxide for electrochemical sensing.

    PubMed

    Dong, Wenhao; Ren, Yipeng; Zhang, Yanyan; Chen, Yuan; Zhang, Cong; Bai, Zhixue; Ma, Rui; Chen, Qiang

    2017-04-01

    Graphene sheets are a sp(2)-hybridized carbon material that offer extraordinary electrical conductivity and excellent thermal and mechanical properties. They are expected to find use in a wide variety of applications. In this study, a new novel electrocatalyst, a Pb nanowires-Au nanoparticles nanocomposite decorated with reduced graphene oxide (rGO-Pb NWs-Au NPs), was successfully synthesized by an effective and simple approach. Transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman spectroscopy were employed to observe the as-prepared nanomaterial. In addition, the electrochemical behaviors of a rGO-Pb NWs-Au NPs-modified glassy carbon (GC) electrode were evaluated by cyclic voltammetry and chronoamperometry. The final prepared sensor exhibited favorable electroreduction activity towards H2O2 with a remarkable sensitivity of 552.43µAmM(-1)cm(-2), a wide linear range of 0.005-1.25mM, a detection limit of 0.6µM and a rapid response time (within 5s). Moreover, the sensor also exhibited good reproducibility, selectivity and stability. Therefore, the present work also provides a potential practicable approach to fabricate various of non-enzymatic amperometric sensors, such as sensors for the detection of glucose, urea, ascorbic acid and dopamine.

  15. Characterisation of reduced graphene oxides prepared from natural flaky, lump and amorphous graphites

    SciTech Connect

    Peng, Weijun; Li, Hongqiang Hu, Yang; Liu, Yanyan; Song, Shaoxian

    2016-06-15

    Highlights: • Natural flaky, lumpy and amorphous graphites were used to synthesis rGO. • Investigation the effect of the crystal morphology on the oxidation process of GrO and characteristics of prepared rGO. • Low graphitisation degree, big specific surface area and small lateral size were beneficial to the oxidation of graphite. - Abstract: The characterisation of reduced graphene oxides (rGOs) prepared from natural flaky, lumpy, and amorphous graphites using Hummers method was investigated. The prepared graphite oxides (GrOs) and rGOs were characterised by X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, UV–vis spectroscopy, atomic force microscopy and electrochemical performance. The results showed that amorphous graphite was much easier to oxidise than lumpy and flaky graphites and was preferable for preparing single or double layer graphene because low graphitisation degree, high defect degree, high specific surface area and small crystal size were beneficial for (1) the oxidants to attack the exposed carbon atoms, (2) the intercalation of oxidants, and (3) the diffusion of oxidants between graphitic layers. In addition, rGO synthesised from amorphous graphite had the most defects and the smallest size of the in-plane sp{sup 2} domains compared to those obtained from the other two nature graphites.

  16. Ceria and copper/ceria functional coatings for electrochemical applications: Materials preparation and characterization

    NASA Astrophysics Data System (ADS)

    Melnik, J.; Fu, X. Z.; Luo, J. L.; Sanger, A. R.; Chuang, K. T.; Yang, Q. M.

    Following preliminary investigations, two electrodeposition techniques (electrophoretic and electrolytic) were selected and adapted for deposition of doped ceria ceramic and copper/doped ceria composite coatings on Ni substrates (foil and foam). The copper/doped ceria composites have potential value as protective functional coatings for current collectors in electrochemical cells including solid oxide fuel sells (SOFC). The doped ceria ceramic coating has potential application as a porous matrix for anodes of SOFCs operating on syngas, sour gas, or hydrocarbons.

  17. Method of preparing a powdered, electrically insulative separator for use in an electrochemical cell

    DOEpatents

    Cooper, Tom O.; Miller, William E.

    1978-01-01

    A secondary electrochemical cell includes electrodes separated by a layer of electrically insulative powder. The powder includes refractory materials selected from the oxides and nitrides of metals and metaloids. The powdered refractory material, blended with electrolyte particles, is compacted as layers onto an electrode to form an integral electrode structure and assembled into the cell. The assembled cell is heated to its operating temperature leaving porous layers of electrically insulative, refractory particles, containing molten electrolyte between the electrodes.

  18. Electrochemical and spectroscopic studies of the oxidation mechanism of the herbicide propanil.

    PubMed

    Garrido, E M; Lima, J L F C; Delerue-Matos, C; Borges, F; Silva, A M S; Piedade, J A P; Oliveira Brett, A M

    2003-02-12

    Electrochemical oxidation of propanil in deuterated solutions was studied by cyclic, differential pulse, and square wave voltammetry using a glassy carbon microelectrode. The oxidation of propanil in deuterated acid solutions occurs at the nitrogen atom of the amide at a potential of +1.15 V vs Ag/AgCl. It was also found that, under the experimental conditions used, protonation at the oxygen atom of propanil occurs, leading to the appearance of another species in solution which oxidizes at +0.60 V. The anodic peak found at +0.79 V vs Ag/AgCl in deuterated basic solutions is related to the presence of an anionic species in which a negative charge is on the nitrogen atom. The electrochemical data were confirmed by the identification of all the species formed in acidic and basic deuterated solutions by means of NMR spectroscopy. The results are supported by electrochemical and spectroscopic studies of acetanilide in deuterated solutions.

  19. Combining Electrochemical Sensors with Miniaturized Sample Preparation for Rapid Detection in Clinical Samples

    PubMed Central

    Bunyakul, Natinan; Baeumner, Antje J.

    2015-01-01

    Clinical analyses benefit world-wide from rapid and reliable diagnostics tests. New tests are sought with greatest demand not only for new analytes, but also to reduce costs, complexity and lengthy analysis times of current techniques. Among the myriad of possibilities available today to develop new test systems, amperometric biosensors are prominent players—best represented by the ubiquitous amperometric-based glucose sensors. Electrochemical approaches in general require little and often enough only simple hardware components, are rugged and yet provide low limits of detection. They thus offer many of the desirable attributes for point-of-care/point-of-need tests. This review focuses on investigating the important integration of sample preparation with (primarily electrochemical) biosensors. Sample clean up requirements, miniaturized sample preparation strategies, and their potential integration with sensors will be discussed, focusing on clinical sample analyses. PMID:25558994

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

    PubMed Central

    Gergin, İlknur; Ismar, Ezgi

    2017-01-01

    In this study, a precursor for carbon nanofibers (CNF) was fabricated via electrospinning and carbonized through a thermal process. Before carbonization, oxidative stabilization should be applied, and the oxidation mechanism also plays an important role during carbonization. Thus, the understanding of the oxidation mechanism is an essential part of the production of CNF. The oxidation process of polyacrylonitrile was studied and nanofiber webs containing graphene oxide (GO) are obtained to improve the electrochemical properties of CNF. Structural and morphological characterizations of the webs are carried out by using attenuated total reflectance Fourier transform infrared spectroscopy and Raman spectroscopy, scanning electron microscopy, atomic force microscopy and transmission electron microscopy. Mechanical tests are performed with a dynamic mechanical analyzer, and thermal studies are conducted by using thermogravimetric analysis. Electrochemical impedance spectroscopy, and cyclic voltammetry are used to investigate capacitive behavior of the products. The proposed equivalent circuit model was consistent with charge-transfer processes taking place at interior pores filled with electrolyte. PMID:28875098

  1. Silver Vanadium Phosphorous Oxide, Ag(2)VO(2)PO(4): Chimie Douce Preparation and Resulting Lithium Cell Electrochemistry.

    PubMed

    Kim, Young Jin; Marschilok, Amy C; Takeuchi, Kenneth J; Takeuchi, Esther S

    2011-08-15

    Recently, we have shown silver vanadium phosphorous oxide (Ag(2)VO(2)PO(4), SVPO) to be a promising cathode material for lithium based batteries. Whereas the first reported preparation of SVPO employed an elevated pressure, hydrothermal approach, we report herein a novel ambient pressure synthesis method to prepare SVPO, where our chimie douce preparation is readily scalable and provides material with a smaller, more consistent particle size and higher surface area relative to SVPO prepared via the hydrothermal method. Lithium electrochemical cells utilizing SVPO cathodes made by our new process show improved power capability under constant current and pulse conditions over cells containing cathode from SVPO prepared via the hydrothermal method.

  2. Silver vanadium phosphorous oxide, Ag 2VO 2PO 4: Chimie douce preparation and resulting lithium cell electrochemistry

    NASA Astrophysics Data System (ADS)

    Kim, Young Jin; Marschilok, Amy C.; Takeuchi, Kenneth J.; Takeuchi, Esther S.

    Recently, we have shown silver vanadium phosphorous oxide (Ag 2VO 2PO 4, SVPO) to be a promising cathode material for lithium based batteries. Whereas the first reported preparation of SVPO employed an elevated pressure, hydrothermal approach, we report herein a novel ambient pressure synthesis method to prepare SVPO, where our chimie douce preparation is readily scalable and provides material with a smaller, more consistent particle size and higher surface area relative to SVPO prepared via the hydrothermal method. Lithium electrochemical cells utilizing SVPO cathodes made by our new process show improved power capability under constant current and pulse conditions over cells containing cathode from SVPO prepared via the hydrothermal method.

  3. Remediation of a winery wastewater combining aerobic biological oxidation and electrochemical advanced oxidation processes.

    PubMed

    Moreira, Francisca C; Boaventura, Rui A R; Brillas, Enric; Vilar, Vítor J P

    2015-05-15

    Apart from a high biodegradable fraction consisting of organic acids, sugars and alcohols, winery wastewaters exhibit a recalcitrant fraction containing high-molecular-weight compounds as polyphenols, tannins and lignins. In this context, a winery wastewater was firstly subjected to a biological oxidation to mineralize the biodegradable fraction and afterwards an electrochemical advanced oxidation process (EAOP) was applied in order to mineralize the refractory molecules or transform them into simpler ones that can be further biodegraded. The biological oxidation led to above 97% removals of dissolved organic carbon (DOC), chemical oxygen demand (COD) and 5-day biochemical oxygen demand (BOD5), but was inefficient on the degradation of a bioresistant fraction corresponding to 130 mg L(-1) of DOC, 380 mg O2 L(-1) of COD and 8.2 mg caffeic acid equivalent L(-1) of total dissolved polyphenols. Various EAOPs such as anodic oxidation with electrogenerated H2O2 (AO-H2O2), electro-Fenton (EF), UVA photoelectro-Fenton (PEF) and solar PEF (SPEF) were then applied to the recalcitrant effluent fraction using a 2.2 L lab-scale flow plant containing an electrochemical cell equipped with a boron-doped diamond (BDD) anode and a carbon-PTFE air-diffusion cathode and coupled to a photoreactor with compound parabolic collectors (CPCs). The influence of initial Fe(2+) concentration and current density on the PEF process was evaluated. The relative oxidative ability of EAOPs increased in the order AO-H2O2 < EF < PEF ≤ SPEF. The SPEF process using an initial Fe(2+) concentration of 35 mg L(-1), current density of 25 mA cm(-2), pH of 2.8 and 25 °C reached removals of 86% on DOC and 68% on COD after 240 min, regarding the biologically treated effluent, along with energy consumptions of 45 kWh (kg DOC)(-1) and 5.1 kWh m(-3). After this coupled treatment, color, odor, COD, BOD5, NH4(+), NO3(-) and SO4(2-) parameters complied with the legislation targets and, in addition, a total

  4. Preparation and Characterization of Graphene Oxide Paper

    SciTech Connect

    Dikin,D.; Stankovich, S.; Zimney, E.; Piner, R.; Dommett, G.; Evmenenko, G.; Nguyen, S.; Ruoff, R.

    2007-01-01

    Free-standing paper-like or foil-like materials are an integral part of our technological society. Their uses include protective layers, chemical filters, components of electrical batteries or supercapacitors, adhesive layers, electronic or optoelectronic components, and molecular storage. Inorganic 'paper-like' materials based on nanoscale components such as exfoliated vermiculite or mica platelets have been intensively studied and commercialized as protective coatings, high-temperature binders, dielectric barriers and gas-impermeable membranes. Carbon-based flexible graphite foils composed of stacked platelets of expanded graphite have long been used in packing and gasketing applications because of their chemical resistivity against most media, superior sealability over a wide temperature range, and impermeability to fluids. The discovery of carbon nanotubes brought about bucky paper, which displays excellent mechanical and electrical properties that make it potentially suitable for fuel cell and structural composite applications. Here we report the preparation and characterization of graphene oxide paper, a free-standing carbon-based membrane material made by flow-directed assembly of individual graphene oxide sheets. This new material outperforms many other paper-like materials in stiffness and strength. Its combination of macroscopic flexibility and stiffness is a result of a unique interlocking-tile arrangement of the nanoscale graphene oxide sheets.

  5. Review on landfill leachate treatment by electrochemical oxidation: Drawbacks, challenges and future scope.

    PubMed

    Mandal, Pubali; Dubey, Brajesh K; Gupta, Ashok K

    2017-08-30

    Various studies on landfill leachate treatment by electrochemical oxidation have indicated that this process can effectively reduce two major pollutants present in landfill leachate; organic matter and ammonium nitrogen. In addition, the process is able to enhance the biodegradability index (BOD/COD) of landfill leachate, which make mature or stabilized landfill leachate suitable for biological treatment. The elevated concentration of ammonium nitrogen especially observed in bioreactor landfill leachate can also be reduced by electrochemical oxidation. The pollutant removal efficiency of the system depends upon the mechanism of oxidation (direct or indirect oxidation) which depends upon the property of anode material. Applied current density, pH, type and concentration of electrolyte, inter-electrode gap, mass transfer mode, total anode area to volume of effluent to be treated ratio, temperature, flow rate or flow velocity, reactor geometry, cathode material and lamp power during photoelectrochemical oxidation may also influence the system performance. In this review paper, past and present scenarios of landfill leachate treatment efficiencies and costs of various lab scale, pilot scale electrochemical oxidation studies asa standalone system or integrated with biological and physicochemical processes have been reviewed with the conclusion that electrochemical oxidation can be employed asa complementary treatment system with biological process for conventional landfill leachate treatment as well asa standalone system for ammonium nitrogen removal from bioreactor landfill leachate. Furthermore, present drawbacks of electrochemical oxidation process asa landfill leachate treatment system and relevance of incorporating life cycle assessment into the decision-making process besides process efficiency and cost, have been discussed. Copyright © 2017 Elsevier Ltd. All rights reserved.

  6. Great-enhanced performance of Pt nanoparticles by the unique carbon quantum dot/reduced graphene oxide hybrid supports towards methanol electrochemical oxidation

    NASA Astrophysics Data System (ADS)

    Hong, Tian-Zeng; Xue, Qiong; Yang, Zhi-Yong; Dong, Ya-Ping

    2016-01-01

    The Pt-carbon quantum dot (CQD)/reduced graphene oxide (RGO) catalysts are prepared by one pot reduction method and demonstrate ultraefficient performance towards methanol oxidation reaction (MOR). In the high content CQD products, Pt nanoparticles around 2-3 nm are dispersed uniformly on supporting materials. And the X-ray photoelectron spectroscopy analysis indicates that in the high content CQD products a large part of surface oxygen groups is contributed by CQD. The electrochemical tests reveal that the catalyst with the saturated CQD exhibits best performance in MOR: the mass and specific activity at forward peak position, the potential close to fuel cell operation and 3600 s of chronoamperometric curve are roughly 2-3 folds of the commercial Pt/C. Furthermore, the electrochemical data on the series of catalysts with different quantity of CQD disclose the improving tendency of MOR performance with the increasing content of CQD evidently. Overview the electrochemical and characterization results, we suggest CQD play multiple roles in the enhancement of Pt performance: present abundant nucleating and anchoring points to facilitate the formation of small size and uniform distributed Pt particles; act as spacer to alleviate restacking of RGO sheets; and provide fruitful surface oxygen groups to improve the antipoisonous ability of Pt.

  7. Electrochemical oxidation of 2,4,5-trichlorophenoxyacetic acid by metal-oxide-coated Ti electrodes.

    PubMed

    Maharana, Dusmant; Xu, Zesheng; Niu, Junfeng; Rao, Neti Nageswara

    2015-10-01

    Electrochemical oxidation of 2,4,5-trichlorophenoxyacetic acid (2,4,5-T) over metal-oxide-coated Ti anodes, i.e., Ti/SnO2-Sb/Ce-PbO2, Ti/SnO2-Sb and Ti/RuO2, was examined. The degradation efficiency of over 90% was attained at 20 min at different initial concentrations (0.5-20 mg L(-1)) and initial pH values (3.1-11.2). The degradation efficiencies of 2,4,5-T on Ti/SnO2-Sb/Ce-PbO2, Ti/SnO2-Sb and Ti/RuO2 anodes were higher than 99.9%, 97.2% and 91.5% at 30 min, respectively, and the respective total organic carbon removal ratios were 65.7%, 54.6% and 37.2%. The electrochemical degradation of 2,4,5-T in aqueous solution followed pseudo-first-order kinetics. The compounds, i.e., 2,5-dichlorohydroquinone and 2,5-dihydroxy-p-benzoquinone, have been identified as the main aromatic intermediates by liquid chromatography-mass spectrometry. The results showed that the energy efficiencies of 2,4,5-T (20 mg L(-1)) degradation with Ti/SnO2-Sb/Ce-PbO2 anode at the optimal current densities from 2 to 16 mA cm(-2) ranged from 8.21 to 18.73 kWh m(-3). Copyright © 2015 Elsevier Ltd. All rights reserved.

  8. Mediated electrochemical oxidation of organic wastes without electrode separators

    DOEpatents

    Farmer, J.C.; Wang, F.T.; Hickman, R.G.; Lewis, P.R.

    1996-05-14

    An electrochemical cell/electrolyte/mediator combination is described for the efficient destruction of organic contaminants using metal salt mediators in a sulfuric acid electrolyte, wherein the electrodes and mediator are chosen such that hydrogen gas is produced at the cathode and no cell membrane is required. 3 figs.

  9. Mediated electrochemical oxidation of organic wastes without electrode separators

    DOEpatents

    Farmer, Joseph C.; Wang, Francis T.; Hickman, Robert G.; Lewis, Patricia R.

    1996-01-01

    An electrochemical cell/electrolyte/mediator combination for the efficient destruction of organic contaminants using metal salt mediators in a sulfuric acid electrolyte, wherein the electrodes and mediator are chosen such that hydrogen gas is produced at the cathode and no cell membrane is required.

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

    SciTech Connect

    Gupta, Vinay Kawaguchi, Toshikazu; Miura, Norio

    2009-01-08

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

  11. Electrochemical oxidation of wine polyphenols in the presence of sulfur dioxide.

    PubMed

    Makhotkina, Olga; Kilmartin, Paul A

    2013-06-12

    Electrochemical oxidation of three representative wine polyphenols (catechin, caffeic acid, and quercetin) in the presence of sulfur dioxide in a model wine solution (pH = 3.3) was investigated. The oxidation was undertaken using chronoamperometry at a rotating glassy carbon rod electrode, and the reaction products were characterized by HPLC-MS. The mechanism of electrochemical oxidation of polyphenols in the presence of sulfur dioxide was proposed to be an ECEC mechanism. The polyphenols first underwent a one-electron oxidation to a semiquinone radical, which can be reduced back to the original polyphenol by sulfur dioxide, or further oxidized to the quinone form. In the cases of caffeic acid and catechin, the quinone combined with sulfur dioxide and produced new derivatives. The quercetin quinone underwent further chemical transformations, producing several new compounds. The proposed mechanisms were confirmed by digital simulation of cyclic voltammograms.

  12. Nanoscale electrochemical patterning reveals the active sites for catechol oxidation at graphite surfaces.

    PubMed

    Patel, Anisha N; McKelvey, Kim; Unwin, Patrick R

    2012-12-19

    Graphite-based electrodes (graphite, graphene, and nanotubes) are used widely in electrochemistry, and there is a long-standing view that graphite step edges are needed to catalyze many reactions, with the basal surface considered to be inert. In the present work, this model was tested directly for the first time using scanning electrochemical cell microscopy reactive patterning and shown to be incorrect. For the electro-oxidation of dopamine as a model process, the reaction rate was measured at high spatial resolution across a surface of highly oriented pyrolytic graphite. Oxidation products left behind in a pattern defined by the scanned electrochemical cell served as surface-site markers, allowing the electrochemical activity to be correlated directly with the graphite structure on the nanoscale. This process produced tens of thousands of electrochemical measurements at different locations across the basal surface, unambiguously revealing it to be highly electrochemically active, with step edges providing no enhanced activity. This new model of graphite electrodes has significant implications for the design of carbon-based biosensors, and the results are additionally important for understanding electrochemical processes on related sp(2)-hybridized materials such as pristine graphene and nanotubes.

  13. Electrochemical and photoelectrochemical oxidation of 5-hydroxymethylfurfural to 2,5-furandicarboxylic acid and 2,5-diformylfuran

    DOEpatents

    Choi, Kyoung-Shin; Cha, Hyun Gil

    2017-03-21

    Electrochemical and photoelectrochemical cells for the oxidation of 5-hydroxymethylfurfural to 2,5-furandicarboxylic acid and/or 2,5-diformylfuran are provided. Also provided are methods of using the cells to carry out the electrochemical and photoelectrochemical oxidation of 5-hydroxymethylfurfural to 2,5-furandicarboxylic acid and/or 2,5-diformylfuran.

  14. Note: Buoyant-force assisted liquid membrane electrochemical etching for nano-tip preparation

    NASA Astrophysics Data System (ADS)

    Zeng, Yongbin; Wang, Yufeng; Wu, Xiujuan; Xu, Kun; Qu, Ningsong

    2014-12-01

    A liquid membrane electrochemical etching process for preparing nano-tips is proposed by the introduction of buoyant force to the lower tip, in which the lower portion of the anodic wire is immersed into a floating layer. A mathematical model of this method is derived. Both calculation and experimental results demonstrate that the introduction of buoyant force can significantly decrease the tip radius. The lubricating oil and deionized water floating layers were tested for the processing of nano-tips. Further, high-aspect-ratio nano-electrodes were prepared by applying a relative vertical movement to the anodic wire.

  15. Electrochemical synthesis of nickel-aluminium oxide system from metals obtained by ore processing

    NASA Astrophysics Data System (ADS)

    Korobochkin, V. V.; Usoltseva, N. V.; Shorokhov, K. G.; Popova, E. V.

    2015-11-01

    Separate and combined electrochemical oxidation of aluminium and nickel has been conducted by alternating current of industrial frequency. Concentration increase of electrolyte solution (sodium chloride) in the range from 3 to 25 wt. % and current density from 0.5 to 1.5 A/cm2 was found to result in the increasing metal oxidation rate, excluding aluminium oxidation which oxidation rate is independent of the electrolyte solution concentration. At the current density of 1.5 A/cm2 the products of separate oxidation of nickel and aluminium are nickel oxyhydroxides, nickel hydroxides and aluminium oxyhydroxide (boehmite), respectively. In addition to these compounds, the nickel-aluminium oxide hydrate is included in the products of nickel and aluminium co-oxidation. Its content grows with the increasing electrolyte solution concentration. Varying the concentration and current density within the limits indicated, the nickel-aluminium oxide system with nickel oxide content from 3 to 10 wt. % is produced.

  16. Annealing of indium tin oxide (ITO) coated optical fibers for optical and electrochemical sensing purposes

    NASA Astrophysics Data System (ADS)

    Dominik, Magdalena; Siuzdak, Katarzyna; Niedziałkowski, Paweł; Stranak, Vitezslav; Sezemsky, Petr; Sobaszek, Michał; Bogdanowicz, Robert; Ossowski, Tadeusz; Śmietana, Mateusz

    2016-12-01

    Glass and fiber structures with Indium Tin Oxide (ITO) coating were subjected to annealing in order to identify impact of the thermal treatment on their optical and electrochemical properties. It is shown that the annealing process significantly modifies optical properties and thickness of the films, which are crucial for performance of optical fiber sensors. Moreover, it visibly improves electrochemical activity of ITO on glass slides and thicker (∅=400 μm) ITO-coated fibers, whereas in the case of thinner fibers (∅=125 μm) it could lead to a loss of their electrochemical activity. Depending on the applied substrate and the annealing process, the investigated structures with ITO coating can be further used as fiber-based sensors with integrated opto-electrochemical readout.

  17. Effect of nanostructured graphene oxide on electrochemical activity of its composite with polyaniline titanium dioxide

    NASA Astrophysics Data System (ADS)

    Binh Phan, Thi; Thanh Luong, Thi; Mai, Thi Xuan; Thanh Thuy Mai, Thi; Tot Pham, Thi

    2016-03-01

    Graphene oxide (GO) significantly affects the electrochemical activity of its composite with polyanline titanium dioxide (TiO2). In this work various composites with different GO contents have been successfully synthesized by chemical method to compare not only their material properties but also electrochemical characteristics with each other. The results of an electrochemical impedance study showed that their electrochemical property has been improved due to the presence of GO in a composite matrix. The galvanodynamic polarization explained that among them the composite with GO/Ani ratio in the range of 1-14 exhibits a better performance compared to the other due to yielding a higher current desity (280 μA cm-2). The TEM and SEM images which presented the fibres of a composite bundle with the presence of PANi and TiO2 were examined by IR-spectra and x-ray diffraction, respectively.

  18. Integrating electrochemical oxidation into forward osmosis process for removal of trace antibiotics in wastewater.

    PubMed

    Liu, Pengxiao; Zhang, Hanmin; Feng, Yujie; Shen, Chao; Yang, Fenglin

    2015-10-15

    During the rejection of trace pharmaceutical contaminants from wastewater by forward osmosis (FO), disposal of the FO concentrate was still an unsolved issue. In this study, by integrating the advantages of forward osmosis and electrochemical oxidation, a forward osmosis process with the function of electrochemical oxidation (FOwEO) was established for the first time to achieve the aim of rejection of trace antibiotics from wastewater and treatment of the concentrate at the same time. Results demonstrated that FOwEO (current density J=1 mA cm(-2)) exhibited excellent rejections of antibiotics (>98%) regardless of different operation conditions, and above all, antibiotics in the concentrate were well degraded (>99%) at the end of experiment (after 3h). A synergetic effect between forward osmosis and electrochemical oxidation was observed in FOwEO, which lies in that antibiotic rejections by FO were enhanced due to the degradation of antibiotics in the concentrate, while the electrochemical oxidation capacity was improved in the FOwEO channel, of which good mass transfer and the assist of indirect oxidation owing to the reverse NaCl from draw solution were supposed to be the mechanism. This study demonstrated that the FOwEO has the capability to thoroughly remove trace antibiotics from wastewater. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Porous nanoarchitectures of spinel-type transition metal oxides for electrochemical energy storage systems.

    PubMed

    Park, Min-Sik; Kim, Jeonghun; Kim, Ki Jae; Lee, Jong-Won; Kim, Jung Ho; Yamauchi, Yusuke

    2015-12-14

    Transition metal oxides possessing two kinds of metals (denoted as AxB3-xO4, which is generally defined as a spinel structure; A, B = Co, Ni, Zn, Mn, Fe, etc.), with stoichiometric or even non-stoichiometric compositions, have recently attracted great interest in electrochemical energy storage systems (ESSs). The spinel-type transition metal oxides exhibit outstanding electrochemical activity and stability, and thus, they can play a key role in realising cost-effective and environmentally friendly ESSs. Moreover, porous nanoarchitectures can offer a large number of electrochemically active sites and, at the same time, facilitate transport of charge carriers (electrons and ions) during energy storage reactions. In the design of spinel-type transition metal oxides for energy storage applications, therefore, nanostructural engineering is one of the most essential approaches to achieving high electrochemical performance in ESSs. In this perspective, we introduce spinel-type transition metal oxides with various transition metals and present recent research advances in material design of spinel-type transition metal oxides with tunable architectures (shape, porosity, and size) and compositions on the micro- and nano-scale. Furthermore, their technological applications as electrode materials for next-generation ESSs, including metal-air batteries, lithium-ion batteries, and supercapacitors, are discussed.

  20. Ascorbic Acid Assisted Synthesis of Cobalt Oxide Nanostructures, Their Electrochemical Sensing Application for the Sensitive Determination of Hydrazine

    NASA Astrophysics Data System (ADS)

    Tahira, Aneela; Nafady, Ayman; Baloach, Quarratulain; Sirajuddin; Sherazi, Syed Tufail Hussain; Shaikh, Tayyaba; Arain, Munazza; Willander, Magnus; Ibupoto, Zafar Hussain

    2016-07-01

    This study describes, the synthesis of cobalt oxide nanostructures using ascorbic acid as a growth directing agent by the hydrothermal method. Ascorbic acid is used for the first time for the synthesis of cobalt oxide nanostructures and a unique morphology is prepared in the present study. The cobalt oxide nanostructures were characterized by scanning electron microcopy, x-ray diffraction, and x-ray photoelectron spectroscopy techniques. These analytical techniques demonstrated well defined morphology, good crystalline quality, and high purity of as prepared cobalt oxide nanostructures. The glassy carbon electrode was modified with cobalt oxide nanostructures for the development of a sensitive and selective electrochemical hydrazine sensor. The developed hydrazine sensor exhibits a linear range of 2-24 μM. The sensitivity and limit of detection of presented hydrazine sensors are 12,734 μA/mM/cm2 and 0.1 μM respectively. The developed hydrazine sensor is highly selective, stable, and reproducible. The proposed sensor is successfully applied for the detection of hydrazine from different water samples. The present study provides the development of an alternative tool for the reliable monitoring of hydrazine from environmental and biological samples.

  1. Electrochemical functionalization of polypyrrole through amine oxidation of poly(amidoamine) dendrimers: Application to DNA biosensor.

    PubMed

    Miodek, Anna; Mejri-Omrani, Nawel; Khoder, Rabih; Korri-Youssoufi, Hafsa

    2016-07-01

    Electrochemical patterning method has been developed to fabricate composite based on polypyrrole (PPy) film and poly(amidoamine) dendrimers of fourth generation (PAMAM G4). PPy layer was generated using electrochemical polymerization of pyrrole on a gold electrode. PPy film was then modified with PAMAM G4 using amines electro-oxidation method. Covalent bonding of PAMAM G4 and the formation of PPy-PAMAM composite was characterized using Fourier Transform Infrared Spectroscopy (FT-IR) and X-ray Photoelectron Spectroscopy (XPS). Ferrocenyl groups were then attached to such surface as a redox marker. Electrochemical properties of the modified nanomaterial (PPy-PAMAM-Fc) were studied using both amperometric and impedimetric methods to demonstrate the efficiency of electron transfer through the modified PPy layer. The obtained electrical and electrochemical properties were compared to a composite where PPy bearing carboxylic acid functions was chemically modified with PAMAM G4 by covalent attachment through formation of amid bond (PPy-CONH-PAMAM). The above mentioned studies showed that electrochemical patterning does not disturb the electronic properties of PPy. The effect of the number of functional groups introduced by the electrochemical patterning was demonstrated through the association of various compounds (ethylenediamine, PAMAM G2 and PAMAM G6). We demonstrated that such compounds could be applied in the biosensors technology. The modified PPy-PAMAM-Fc was evaluated as a platform for DNA sensing. High performance in the DNA detection by variation of the electrochemical signal of ferrocene was obtained with detection limit of 0.4 fM. Furthermore, such approach of electrochemical patterning by oxidation of amines could be applied for chemical modification of PPy and open a new way in various biosensing application involving functionalized PPy.

  2. Preparation of Mixed Perovskite Oxides for Blue-Green Lasers

    DTIC Science & Technology

    1984-02-01

    higher for oxide or fluoride . 𔃽. A high radiative lifetime and high fluorescent quantum yield for Ce or the rare earth are desirable. 3 + 4...for all of our single crystal -4- preparations are lanthanum oxide (La„0 ), aluminum oxide (Al^O^) , scandium oxide (Sc„0-.) , and cerium oxide (Ce...crystal material is highly important. Ideally, oxides should be grown in O2, fluorides in ?„, and so forth in order to prevent defects such as

  3. News in Regions of Electrochemical Synthesis of Oxidizers

    DTIC Science & Technology

    of compounds: chlorine oxides, persulfuric acid, ammonium persulfate, manganese oxides, bichromates, bromates, iodates, iodic acid, perborates , percarbonates, and lead tetra-acetate. A bibliography of 95 items is included.

  4. Synthesis and electrochemical capacitance of long tungsten oxide nanorod arrays grown vertically on substrate

    SciTech Connect

    Park, Sun Hwa; Kim, Young Heon; Lee, Tae Geol; Shon, Hyun Kyong; Park, Hyun Min; Song, Jae Yong

    2012-11-15

    Highlights: ► Growth of long amorphous tungsten oxide nanorods on a substrate. ► Formation of single-crystalline tungsten oxide nanorods by a heat-treatment. ► High electrochemical pseudocapacitance of 2.8 mF cm{sup −2}. ► Excellent cyclability of psuedocapacitance up to 1000 cycles. -- Abstract: Long tungsten oxide nanorods are vertically grown on Al/W/Ti coated silicon substrates using a two-step anodization process. The first anodization of the Al film forms a mesh-like mask of anodic aluminum oxide, and the second anodization of the W film results in the formation of a buffer layer, a bottom nanorod, and a top nanorod of amorphous tungsten oxide. A pore-widening process prior to the second anodization leads to the enhancement of nanorod length above approximately 500 nm. After a heat-treatment, the tungsten oxide nanorods are crystallized to form a single crystalline structure while the buffer layer forms a polycrystalline structure. The crystalline tungsten oxide nanorods show a cyclic voltammogram retaining the quasi-rectangular shape of an electrochemically reversible faradaic redox reaction, i.e., a typical pseudocapacitive behavior. The maximum electrochemical capacitance per apparent surface area reaches approximately 2.8 mF cm{sup −2} at the voltage scan rate of 20 mV s{sup −1}, and the excellent cyclability of charge–discharge process is maintained up to 1000 cycles.

  5. Effects of Salts and Metal Oxides on Electrochemical and Optical Properties of Streptococcus mutans

    NASA Astrophysics Data System (ADS)

    Kawai, Tsuyoshi; Nagame, Seigo; Kambara, Masaki; Yoshino, Katsumi

    1994-10-01

    The effects of calcium salts and metal oxide powders on electrochemical, optical and biological properties of Streptococcus mutans have been studied as a novel method to determine the strain. Electrochemical signals of Streptococcus mutans show remarkable decrease in the presence of saturated calcium salts such as CaHPO4, Ca3(PO4)2, and Ca5(PO4)3OH depending on the strains of Streptococcus mutans: Ingbritt, NCTC-10449, or GS-5. The number of viable cells also decreases upon addition of these powders. The effects of metal oxides such as ZnO and BaTiO3 on the electrochemical characteristics and photoluminescence of Streptococcus mutans have also been studied.

  6. In operando studies on the electrochemical oxidation of water mediated by molecular catalysts.

    PubMed

    Hetterscheid, Dennis G H

    2017-09-12

    Homogeneous reactions in general are relatively easy to study with respect to heterogeneous systems since all catalytic sites are uniform and can be addressed simultaneously. The latter feature is fully out of the window in an electrochemical context, where only the few catalytic species that are sufficiently close to the electrode undergo redox reactions. Especially in the water oxidation reaction where harsh reaction conditions are employed, a clear picture of what is the active species, what products are formed, how one can steer this, and how it all depends on the exact reaction conditions is important to be able to fully unravel the key reaction paths. The combination of electrochemical experiments with on-line detection of the catalytic species and reaction products is a powerful approach to successfully address these questions. Recently, a significant progress has been made in on-line studies on molecular water oxidation catalysts during electrochemical experiments. These are reviewed here.

  7. Preparation and characterization of nanostructured NiO/MnO{sub 2} composite electrode for electrochemical supercapacitors

    SciTech Connect

    Liu Enhui Li Wen; Li Jian; Meng Xiangyun; Ding Rui; Tan Songting

    2009-05-06

    Nanostructured nickel-manganese oxides composite was prepared by the sol-gel and the chemistry deposition combination new route. The surface morphology and structure of the composite were characterized by scanning electron microscope and X-ray diffraction. The as-synthesized NiO/MnO{sub 2} samples exhibit higher surface area of 130-190 m{sup 2} g{sup -1}. Cyclic voltammetry and galvanostatic charge/discharge measurements were applied to investigate the electrochemical performance of the composite electrodes with different ratios of NiO/MnO{sub 2}. When the mass ratio of MnO{sub 2} and NiO in composite material is 80:20, the specific capacitance value of NiO/MnO{sub 2} calculated from the cyclic voltammetry curves is 453 F g{sup -1}, for pure NiO and MnO{sub 2} are 209, 330 F g{sup -1} in 6 mol L{sup -1} KOH electrolyte and at scan rate of 10 mV s{sup -1}, respectively. The specific capacitance of NiO/MnO{sub 2} electrode is much larger than that of each pristine component. Moreover, the composite electrodes showed high power density and stable electrochemical properties.

  8. Chemical composition and direct electrochemical oxidation of table olive processing wastewater using high oxidation power anodes.

    PubMed

    Gargouri, Boutheina; Gargouri, Olfa Dridi; Khmakhem, Ibtihel; Ammar, Sonda; Abdelhèdi, Ridha; Bouaziz, Mohamed

    2017-01-01

    Table olive processing wastewater (TOW) is a notoriously polluting due to its high organic and phenol content. To reduce them, an electrochemical process has been studied for the treatment of this effluent. Experiments were performed with a cell equipped with lead dioxide (PbO2) or boron-doped diamond (BDD) as anode and platinum as cathode, where Table Olive Wastewater (TOW) were destroyed by hydroxyl radicals formed at the anode surface from water oxidation. The comparative study of both systems shows the performance of the BDD anode compared to PbO2, explained by the large amounts of hydroxyl radicals generated effective at BDD anode and its synthesis characteristics. Using LC/MS analysis, it was possible to determine hydroxytyrosol, as major phenolic compounds, in table olive processing wastewater and its concentration reach 890 mg L(-1). A possible reaction mechanism oxidation for hydroxytyrosol was proposed. The kinetics decays for hydroxytyrosol degradation on PbO2 anode follows a pseudo-first order reaction with a rate constant 0.9 h(-1) for japp value 20 mA cm(-2).

  9. Nanostructured Mn-based oxides for electrochemical energy storage and conversion.

    PubMed

    Zhang, Kai; Han, Xiaopeng; Hu, Zhe; Zhang, Xiaolong; Tao, Zhanliang; Chen, Jun

    2015-02-07

    Batteries and supercapacitors as electrochemical energy storage and conversion devices are continuously serving for human life. The electrochemical performance of batteries and supercapacitors depends in large part on the active materials in electrodes. As an important family, Mn-based oxides have shown versatile applications in primary batteries, secondary batteries, metal-air batteries, and pseudocapacitors due to their high activity, high abundance, low price, and environmental friendliness. In order to meet future market demand, it is essential and urgent to make further improvements in energy and power densities of Mn-based electrode materials with the consideration of multiple electron reaction and low molecular weight of the active materials. Meanwhile, nanomaterials are favourable to achieve high performance by means of shortening the ionic diffusion length and providing large surface areas for electrode reactions. This article reviews the recent efforts made to apply nanostructured Mn-based oxides for batteries and pseudocapacitors. The influence of structure, morphology, and composition on electrochemical performance has been systematically summarized. Compared to bulk materials and notable metal catalysts, nanostructured Mn-based oxides can promote the thermodynamics and kinetics of the electrochemical reactions occurring at the solid-liquid or the solid-liquid-gas interface. In particular, nanostructured Mn-based oxides such as one-dimensional MnO2 nanostructures, MnO2-conductive matrix nanocomposites, concentration-gradient structured layered Li-rich Mn-based oxides, porous LiNi0.5Mn1.5O4 nanorods, core-shell structured LiMnSiO4@C nanocomposites, spinel-type Co-Mn-O nanoparticles, and perovskite-type CaMnO3 with micro-nano structures all display superior electrochemical performance. This review should shed light on the sustainable development of advanced batteries and pseudocapacitors with nanostructured Mn-based oxides.

  10. PREPARATION OF HIGH-DENSITY, COMPACTIBLE THORIUM OXIDE PARTICLES

    DOEpatents

    McCorkle, K.H.; Kleinsteuber, A.T.; Schilling, C.E.; Dean, O.C.

    1962-05-22

    A method is given for preparing millimeter-size, highdensity thorium oxide particles suitable for fabrication into nuclear reactor feel elements by means of vibratory compaction. A thorium oxide gel containing 3.7 to 7 weight per cent residual volatile nitrate and water is prepared by drying a thorium oxide sol. The gel is then slowly heated to a temperature of about 450DEC, and the resulting gel fragments are calcined. The starting sol is prepared by repeated dispersion of oxalate-source thorium oxide in a nitrate system or by dispersion of steam-denitrated thorium oxide in water. (AEC)

  11. Influence of substrate preparation on the shaping of the topography of the surface of nanoceramic oxide layers

    NASA Astrophysics Data System (ADS)

    Bara, Marek; Kubica, Marek

    2014-02-01

    The paper discusses the shaping mechanism and changes occurring in the structure and topography of the surface of nanoceramic oxide layers during their formation. The paper presents the influence of substrate preparation on the surface topography of oxide layers. The layers were produced via hard anodizing on the EN AW-5251 aluminum alloy. The layers obtained were subjected to microscope examinations, image and chemical composition analyses, and stereometric examinations. Heredity of substrate properties in the topography of the surface of nanoceramic oxide layers formed as a result of electrochemical oxidation has been shown.

  12. Preparation and electrochemical property of Fe3O4/MWCNT nanocomposite

    NASA Astrophysics Data System (ADS)

    Zhao, Tingkai; Ji, Xianglin; Guo, Xinai; Jin, Wenbo; Dang, Alei; Li, Hao; Li, Tiehu

    2016-06-01

    Ferroferric oxide (Fe3O4)/functionalized multi-walled carbon nanotube (f-MWCNT) nanomaterials were synthesized by chemical deposition & hydrothermal method. Fe3O4/f-MWCNT composites possess the same ferrimagnetism as pure Fe3O4, and the composites will present certain orientation in magnetism. The saturation magnetization (Ms) is about 48.84 emu g-1 and the coercivity (Hc) is 19.19 Oe. The electrochemical analysis displays that the glassy carbon electrode coated with Fe3O4/f-MWCNT composite has a favorable promotion for the electrochemical response of H2O2. This process not only widely improved the redox current of H2O2, but also reduced the overpotential of redox process.

  13. Mercury Underpotential Deposition to Determine Iridium and Iridium Oxide Electrochemical Surface Areas

    SciTech Connect

    Alia, Shaun M.; Hurst, Katherine E.; Kocha, Shyam S.; Pivovar, Bryan S.

    2016-06-02

    Determining the surface areas of electrocatalysts is critical for separating the key properties of area-specific activity and electrochemical surface area from mass activity. Hydrogen underpotential deposition and carbon monoxide oxidation are typically used to evaluate iridium (Ir) surface areas, but are ineffective on oxides and can be sensitive to surface oxides formed on Ir metals. Mercury underpotential deposition is presented in this study as an alternative, able to produce reasonable surface areas on Ir and Ir oxide nanoparticles, and able to produce similar surface areas prior to and following characterization in oxygen evolution. Reliable electrochemical surface areas allow for comparative studies of different catalyst types and the characterization of advanced oxygen evolution catalysts. Lastly, they also enable the study of catalyst degradation in durability testing, both areas of increasing importance within electrolysis and electrocatalysis.

  14. Mercury Underpotential Deposition to Determine Iridium and Iridium Oxide Electrochemical Surface Areas

    DOE PAGES

    Alia, Shaun M.; Hurst, Katherine E.; Kocha, Shyam S.; ...

    2016-06-02

    Determining the surface areas of electrocatalysts is critical for separating the key properties of area-specific activity and electrochemical surface area from mass activity. Hydrogen underpotential deposition and carbon monoxide oxidation are typically used to evaluate iridium (Ir) surface areas, but are ineffective on oxides and can be sensitive to surface oxides formed on Ir metals. Mercury underpotential deposition is presented in this study as an alternative, able to produce reasonable surface areas on Ir and Ir oxide nanoparticles, and able to produce similar surface areas prior to and following characterization in oxygen evolution. Reliable electrochemical surface areas allow for comparativemore » studies of different catalyst types and the characterization of advanced oxygen evolution catalysts. Lastly, they also enable the study of catalyst degradation in durability testing, both areas of increasing importance within electrolysis and electrocatalysis.« less

  15. Excellent electrochemical properties of yolk-shell MoO₃ microspheres formed by combustion of molybdenum oxide-carbon composite microspheres.

    PubMed

    Ko, You Na; Park, Seung Bin; Kang, Yun Chan

    2014-04-01

    Yolk-shell MoO3 microspheres are prepared by a two-step process in which molybdenum oxide-carbon (MoO(x)-C) composite microspheres are first obtained by spray pyrolysis, followed by combustion at 400 °C in air. The yolk-shell microspheres exhibit excellent electrochemical properties and structural stability. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    PubMed

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

    2013-10-01

    We report a new method to convert graphene oxide (GO) to stable colloidal dispersion of reduced graphene oxide nanosheets (RGONS) using sodium diphenylamine sulfonate (SDAS) as a reductant, as well as itself and its redox product as the stabilizer. The as-prepared RGONS have been characterized by X-ray diffraction, Fourier transform infrared spectroscopy, UV-visible spectroscopy, thermo-gravimetric analysis, scanning and transmission electron microscopy, X-ray photoelectron spectroscopy, atomic force microscopy and Raman spectroscopy. The results indicate that the bulk of oxygen-containing functional groups from GO have been removed. Based on the cyclic voltammogram (CV) analyses, it is found that the RGONS-based material exhibits better electrochemical activity in sensing ascorbic acid than GO. The simple method provides a new efficient route for the synthesis of water-soluble RGONS on a large scale and novel composites.

  17. Giant third-order nonlinearity from low-loss electrochemical graphene oxide film with a high power stability

    NASA Astrophysics Data System (ADS)

    Ren, Jun; Zheng, Xiaorui; Tian, Zhiming; Li, Dan; Wang, Pu; Jia, Baohua

    2016-11-01

    Giant third-order nonlinear absorption and refraction of electrochemical graphene oxide (EGO) film were investigated in the femtosecond regime using the single beam Z-scan technique. The excellent chemical stability of the EGO film under high-power illumination up to 400 mJ/cm2 is demonstrated, which can be attributed to the low oxidation degree revealed by the optical and Raman spectroscopies. High and broadband linear transmission over 70% has been observed from the visible to the infrared range. The low-loss EGO film with giant third-order nonlinearity, excellent chemical stability, large-scale preparation and flexible integration has a great potential for high-power nonlinear optical applications.

  18. Photo-electrochemical Oxidation of Organic C1 Molecules over WO3 Films in Aqueous Electrolyte: Competition Between Water Oxidation and C1 Oxidation.

    PubMed

    Reichert, Robert; Zambrzycki, Christian; Jusys, Zenonas; Behm, R Jürgen

    2015-11-01

    To better understand organic-molecule-assisted photo-electrochemical water splitting, photo-electrochemistry and on-line mass spectrometry measurements are used to investigate the photo-electrochemical oxidation of the C1 molecules methanol, formaldehyde, and formic acid over WO3 film anodes in aqueous solution and its competition with O2 evolution from water oxidation O2 (+) and CO2 (+) ion currents show that water oxidation is strongly suppressed by the organic species. Photo-electro-oxidation of formic acid is dominated by formation of CO2 , whereas incomplete oxidation of formaldehyde and methanol prevails, with the selectivity for CO2 formation increasing with increasing potential and light intensity. The mechanistic implications for the photo-electro-oxidation of the organic molecules and its competition with water oxidation, which could be derived from this novel approach, are discussed.

  19. Intermediate stages of electrochemical oxidation of single-crystalline platinum revealed by in situ Raman spectroscopy

    PubMed Central

    Huang, Yi-Fan; Kooyman, Patricia J.; Koper, Marc T. M.

    2016-01-01

    Understanding the atomistic details of how platinum surfaces are oxidized under electrochemical conditions is of importance for many electrochemical devices such as fuel cells and electrolysers. Here we use in situ shell-isolated nanoparticle-enhanced Raman spectroscopy to identify the intermediate stages of the electrochemical oxidation of Pt(111) and Pt(100) single crystals in perchloric acid. Density functional theory calculations were carried out to assist in assigning the experimental Raman bands by simulating the vibrational frequencies of possible intermediates and products. The perchlorate anion is suggested to interact with hydroxyl phase formed on the surface. Peroxo-like and superoxo-like two-dimensional (2D) surface oxides and amorphous 3D α-PtO2 are sequentially formed during the anodic polarization. Our measurements elucidate the process of the electrochemical oxidation of platinum single crystals by providing evidence for the structure-sensitive formation of a 2D platinum-(su)peroxide phase. These results may contribute towards a fundamental understanding of the mechanism of degradation of platinum electrocatalysts. PMID:27514695

  20. Advantages of electrodes with dendrimer-protected platinum nanoparticles and carbon nanotubes for electrochemical methanol oxidation.

    PubMed

    Siriviriyanun, Ampornphan; Imae, Toyoko

    2013-04-14

    Electrochemical sensors consisting of electrodes loaded with carbon nanotubes and Pt nanoparticles (PtNPs) protected by dendrimers have been developed using a facile method to fabricate them on two types of disposable electrochemical printed chips with a screen-printed circular gold or a screen-printed circular glassy carbon working electrode. The electrochemical performance of these sensors in the oxidation of methanol was investigated by cyclic voltammetry. It was revealed that such sensors possess stable durability and high electrocatalytic activity: the potential and the current density of an anodic peak in the oxidation of methanol increased with increasing content of PtNPs on the electrodes, indicating the promotion of electrocatalytic activity in relation to the amount of catalyst. The low anodic potential suggests the easy electrochemical reaction, and the high catalyst tolerance supports the almost complete oxidation of methanol to carbon dioxide. The significant performance of these sensors in the detection of methanol oxidation comes from the high electrocatalytic ability of PtNPs, excellent energy transfer of carbon nanotubes and the remarkable ability of dendrimers to act as binders. Thus these systems are effective for a wide range of applications as chemical, biomedical, energy and environmental sensors and as units of direct methanol fuel cells.

  1. Intermediate stages of electrochemical oxidation of single-crystalline platinum revealed by in situ Raman spectroscopy

    NASA Astrophysics Data System (ADS)

    Huang, Yi-Fan; Kooyman, Patricia J.; Koper, Marc T. M.

    2016-08-01

    Understanding the atomistic details of how platinum surfaces are oxidized under electrochemical conditions is of importance for many electrochemical devices such as fuel cells and electrolysers. Here we use in situ shell-isolated nanoparticle-enhanced Raman spectroscopy to identify the intermediate stages of the electrochemical oxidation of Pt(111) and Pt(100) single crystals in perchloric acid. Density functional theory calculations were carried out to assist in assigning the experimental Raman bands by simulating the vibrational frequencies of possible intermediates and products. The perchlorate anion is suggested to interact with hydroxyl phase formed on the surface. Peroxo-like and superoxo-like two-dimensional (2D) surface oxides and amorphous 3D α-PtO2 are sequentially formed during the anodic polarization. Our measurements elucidate the process of the electrochemical oxidation of platinum single crystals by providing evidence for the structure-sensitive formation of a 2D platinum-(su)peroxide phase. These results may contribute towards a fundamental understanding of the mechanism of degradation of platinum electrocatalysts.

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

    PubMed Central

    Filip, Jaroslav; Kasák, Peter; Tkac, Jan

    2016-01-01

    Early diagnostics of diseases performed with minimal money and time consumption has become achievable due to recent advances in development of biosensors. These devices use biorecognition elements for selective interaction with an analyte and signal readout is obtained via different types of transducers. Operational characteristics of biosensors have been reported to improve substantially, when a diverse range of nanomaterials was employed. This review presents construction of electrochemical biosensors based on graphene, atomically thin 2D carbon crystals, which is currently intensively studied nanomaterial. The most attractive directions of graphene applications in biosensor preparation are discussed here including novel detection and amplification schemes exploiting graphene’s unique electrochemical, physical and chemical properties. The future of graphene-based biosensors is most likely bright, but there is still a lot of work to do to fulfill high expectations. PMID:27242391

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

    PubMed

    Filip, Jaroslav; Kasák, Peter; Tkac, Jan

    2015-01-01

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

  4. Electrochemical Preparation of Al-Li-Er-Tm Alloys by Co-reduction

    NASA Astrophysics Data System (ADS)

    Sun, Yi; Zhang, Milin; Han, Wei; Li, Mei; Ye, Ke; Yang, Yusheng; Yan, Yongde; Zhang, Meng

    2013-12-01

    The electrochemical behavior of Al, Li, Er, and Tm was investigated on tungsten electrodes in LiCl-KCl-AlF3-ErCl3-TmCl3 melts. The results indicated that the co-reduction of Al, Li, Er, and Tm occurs at current densities more negative than -0.469 A cm-2 or applied potentials more negative than -2.31 V. The strengthen phases of Al3Er and Al3Tm were prepared by galvanostatic electrolysis and characterized by X-ray diffraction and scanning electron microscopy. ICP-AES analyses showed that the content of lithium, erbium, and thulium in Al-Li-Er-Tm alloys could be controlled by adjusting AlF3 concentration and electrochemical parameters.

  5. Preparation, characterization and PEGylation of superparamagnetic Fe3O4 nanoparticles from ethanol medium via cathodic electrochemical deposition (CED) method

    NASA Astrophysics Data System (ADS)

    Karimzadeh, Isa; Rezagholipour Dizaji, Hamid; Aghazadeh, Mustafa

    2016-09-01

    In this study, we report a practical and effective synthetic method for preparation of naked and polymer coated SPIONs. In this method, naked SPIONs with proper superparamagnetic properties (Ms = 62.9 emu g-1, Mr = 0.75 emu g-1 and Hc = 2.3 Oe) were electrochemically deposited by adjusting optimum electrochemical conditions. Then, polyethylene glycol (PEG) was in situ coated on the SPIONs surface during their electrochemical preparation process. The PEG coat of SPIONs was confirmed by FT-IR, DLS and DSC-TG analyses. The magnetic analysis via VSM revealed that the PEGylated SPIONs have suitable superparamagnetic behavior (Ms = 37.5 emu g-1, Mr = 0.27 emu g-1 and Hc = 1.4 Oe). Based on the obtained results, it was stated that this electrochemical strategy opens a great window for preparation of SPIONs coated with various biocompatible polymers.

  6. Electrochemical fabrication of platinum nanoflakes on fulleropyrrolidine nanosheets and their enhanced electrocatalytic activity and stability for methanol oxidation reaction

    NASA Astrophysics Data System (ADS)

    Zhang, Xuan; Ma, Li-Xia

    2015-07-01

    Pyridine-functionalized fulleropyrrolidine nanosheets are prepared by a fast reprecipitation method under ultrasonication, and used as a novel nanostructured support materials to fabricate Pt catalyst nanoflakes by a simple electrodeposition approach. The as-prepared novel Pt-fullerene hybrid catalyst (Pt/PyC60) exhibits much enhanced electrocatalytic activity and stability for methanol oxidation reaction compared to the unsupported Pt nanoflakes and commercial Pt/C. The introduction of nanostructured fulleropyrrolidine as new support materials not only increases the electrochemically active surface area of catalyst, but also significantly improves the long-term stability. This will contribute to developing functionalized fullerenes as new nanostructured support materials for advanced electrocatalysts in fuel cells.

  7. CO oxidation on stepped-Pt(111) under electrochemical conditions: insights from theory and experiment.

    PubMed

    Busó-Rogero, C; Herrero, E; Bandlow, J; Comas-Vives, A; Jacob, Timo

    2013-11-14

    The co-adsorption of CO and OH on two Pt stepped surfaces vicinal to the (111) orientation has been evaluated by means of density functional theory (DFT) calculations. Focusing on Pt(533) and Pt(221), which contain (100) and (111)-steps, respectively, we find that (111)-steps should be more reactive towards CO oxidation than surfaces containing (100)-steps. The DFT results are compared with electrochemical experiments on the CO adsorption and oxidation on these vicinal surfaces.

  8. Characterization of internal oxide layers in 3% Si grain-oriented steel by electrochemical methods

    SciTech Connect

    Toda, H.; Sato, K.; Komatsubara, M.

    1997-12-01

    The structure of internal oxide layers in decarburized sheet was studied using a newly developed electrochemical method. Dissolving potential profiles indicated the amount of fayalite (Fe{sub 2}SiO{sub 4}) and silica (SiO{sub 2}) in the layers. The quantitative data for the contents of fayalite and silica in the internal oxide layers can be easily obtained by this method.

  9. Poly(4-vinylphenylboronic acid) functionalized polypyrrole/graphene oxide nanosheets for simultaneous electrochemical determination of catechol and hydroquinone

    NASA Astrophysics Data System (ADS)

    Mao, Hui; Liu, Meihong; Cao, Zhenqian; Ji, Chunguang; Sun, Ying; Liu, Daliang; Wu, Shuyao; Zhang, Yu; Song, Xi-Ming

    2017-10-01

    Novel poly(4-vinylphenylboronic acid) (P4VPBA) functionalized polypyrrole/graphene oxide (PPy/GO) nanosheets, which combined the advantages of GO, PPy and PBA groups, were successfully prepared by a simple polymerization of 4-vinylphenylboronic acid (4VPBA) on the surface of pre-treated PPy/GO containing vinyl groups. Because of the synergistic effects of GO with excellent 2D structures and large surface area, PPy with good electronic conductivity and PBA with high recognition capability, P4VPBA/PPy/GO modified glassy carbon electrode presented excellent electrochemical sensing capabilities toward catechol (CC) and hydroquinone (HQ) with good stability, high sensitivity and selectivity, especially giving a large anodic peak potential difference between CC and HQ enough to well distinguish and simultaneously determine the two dihydroxybenzene isomers in their mixture. It is found that PBA groups on the surface of P4VPBA/PPy/GO nanosheets played an essential role for the discrimination and simultaneous electrochemical determination of CC and HQ, which may be due to the selective formation of stable cyclic esters by the covalent interaction between PBA groups and related molecules with a cis-diol in an alkaline aqueous solution. Therefore, P4VPBA/PPy/GO nanosheets can act as a good electrode material for building a steady electrochemical sensor for detecting the two dihydroxybenzene isomers with high sensitivity and selectivity.

  10. Supported Pd-Cu bimetallic nanoparticles that have high activity for the electrochemical oxidation of methanol.

    PubMed

    Yin, Zhen; Zhou, Wu; Gao, Yongjun; Ma, Ding; Kiely, Christopher J; Bao, Xinhe

    2012-04-16

    Monodisperse bimetallic Pd-Cu nanoparticles with controllable size and composition were synthesized by a one-step multiphase ethylene glycol (EG) method. Adjusting the stoichiometric ratio of the Pd and Cu precursors afforded nanoparticles with different compositions, such as Pd(85)-Cu(15), Pd(56)-Cu(44), and Pd(39)-Cu(61). The nanoparticles were separated from the solution mixture by extraction with non-polar solvents, such as n-hexane. Monodisperse bimetallic Pd-Cu nanoparticles with narrow size-distribution were obtained without the need for a size-selection process. Capping ligands that were bound to the surface of the particles were removed through heat treatment when the as-prepared nanoparticles were loaded onto a Vulcan XC-72 carbon support. Supported bimetallic Pd-Cu nanoparticles showed enhanced electrocatalytic activity towards methanol oxidation compared with supported Pd nanoparticles that were fabricated according to the same EG method. For a bimetallic Pd-Cu catalyst that contained 15 % Cu, the activity was even comparable to the state-of-the-art commercially available Pt/C catalysts. A STEM-HAADF study indicated that the formation of random solid-solution alloy structures in the bimetallic Pd(85)-Cu(15)/C catalysts played a key role in improving the electrochemical activity. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Electrochemical immunosensor for ethinylestradiol using diazonium salt grafting onto silver nanoparticles-silica-graphene oxide hybrids.

    PubMed

    Cincotto, Fernando H; Martínez-García, Gonzalo; Yáñez-Sedeño, Paloma; Canevari, Thiago C; Machado, S A S; Pingarrón, José M

    2016-01-15

    This work describes the preparation of an electrochemical immunosensor for ethinylestradiol (EE2) based on grafting of diazonium salt of 4-aminobenzoic acid onto a glassy carbon electrode modified with silver nanoparticles/SiO2/graphene oxide hybrid followed by covalent binding of anti-ethinylestradiol (anti-EE2) to activated carboxyl groups. A competitive immunoassay was developed for the determination of the hormone using peroxidase-labeled ethinylestradiol (HRP-EE2) and measurement of the amperometric response at -200mV in the presence of hydroquinone (HQ) as redox mediator. The calibration curve for EE2 exhibited a linear range between 0.1 and 50ng/mL (r(2)=0.996), with a detection limit of 65pg/mL. Interference studies with other hormones related with EE2 revealed the practical specificity of the developed method for the analyte. A good reproducibility, with RSD=4.5% (n=10) was also observed. The operating stability of a single bioelectrode modified with anti-EE2 was maintained at least for 15 days when it was stored at 4°C under humid conditions between measurements. The developed immunosensor was applied to the analysis of spiked urine with good results.

  12. Ultrasensitive electrochemical immunoassay based on graphene oxide-Ag composites for rapid determination of clenbuterol.

    PubMed

    Bai, Jing; Lai, Yanjun; Jiang, Dawei; Zeng, Yanbo; Xian, Yuezhong; Xiao, Fei; Zhang, Ningdan; Hou, Jie; Jin, Litong

    2012-09-21

    We report the development of an ultrasensitive amperometric biosensor based on Ag nanoparticles-decorated graphene oxide nanosheets (GO) (Ag-GO) for the rapid detection of clenbuterol (CLB). The morphology and structure of the Ag-GO labeled CLB (Ag-GO-CLB) were characterized by transmission electron microscope (TEM), atomic force microscope (AFM), and ultraviolet-visible spectroscope (UV-vis). The immunosensor was prepared by covalently immobilizing capture antibodies on a multi-walled carbon nanotubes-modified glassy carbon electrode. Through competitive immunoreactions, the Ag-GO-CLB nanocomposites were captured on the immunosensor and the silver was measured by positive differential pulse voltammetry (DPV) in KCl solution for the detection of antigen. The experimental results show a linear response over the range from 0.01 to 10.0 ng mL(-1) with a lower detection limit of 6.8 pg mL(-1) (signal-to-noise ratio of 3). The Ag-GO based immunosensor offers a simple and convenient route for metal-immunoassay labels, which can avoid the complicated and time-consuming dissolving of metal component for ultrasensitive determination. Moreover, the electrochemical immunoassay shows acceptable specificity and stability and is suitable for the determination of CLB in real samples.

  13. Application of electrochemically reduced graphene oxide on screen-printed ion-selective electrode.

    PubMed

    Ping, Jianfeng; Wang, Yixian; Ying, Yibin; Wu, Jian

    2012-04-03

    In this study, a novel disposable all-solid-state ion-selective electrode using graphene as the ion-to-electron transducer was developed. The graphene film was prepared on screen-printed electrode directly from the graphene oxide dispersion by a one-step electrodeposition technique. Cyclic voltammetry and electrochemical impedance spectroscopy were employed to demonstrate the large double layer capacitance and fast charge transfer of the graphene film modified electrode. On the basis of these excellent properties, an all-solid-state calcium ion-selective electrode as the model was constructed using the calcium ion-selective membrane and graphene film modified electrode. The mechanism about the graphene promoting the ion-to-electron transformation was investigated in detail. The disposable electrode exhibited a Nernstian slope (29.1 mV/decade), low detection limit (10(-5.8) M), and fast response time (less than 10 s). With the high hydrophobic character of graphene materials, no water film was formed between the ion-selective membrane and the underlying graphene layer. Further studies revealed that the developed electrode was insensitive to light, oxygen, and redox species. The use of the disposable electrode for real sample analysis obtained satisfactory results, which made it a promising alternative in routine sensing applications.

  14. Oxygen vacancy diffusion across cathode/electrolyte interface in solid oxide fuel cells: An electrochemical phase-field model

    NASA Astrophysics Data System (ADS)

    Hong, Liang; Hu, Jia-Mian; Gerdes, Kirk; Chen, Long-Qing

    2015-08-01

    An electrochemical phase-field model is developed to study electronic and ionic transport across the cathode/electrolyte interface in solid oxide fuel cells. The influences of local current density and interfacial electrochemical reactions on the transport behaviors are incorporated. This model reproduces two electrochemical features. Nernst equation is satisfied through the thermodynamic equilibriums of the electron and oxygen vacancy. The distributions of charged species around the interface induce charge double layer. Moreover, we verify the nonlinear current/overpotential relationship. This model facilitates the exploration of problems in solid oxide fuel cells, which are associated with transport of species and electrochemical reactions at high operating temperature.

  15. Chemical and electrochemical study of fabrics coated with reduced graphene oxide

    NASA Astrophysics Data System (ADS)

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

    2013-08-01

    Polyester fabrics coated with reduced graphene oxide (RGO) have been obtained and later characterized by means of chemical and electrochemical techniques. X-ray photoelectron spectroscopy showed a decrease of the oxygen content as well as an increase of the sp2 fraction after chemical reduction of graphene oxide (GO). The electrical conductivity was measured by electrochemical impedance spectroscopy (EIS) and showed a decrease of 5 orders of magnitude in the resistance (Ω) when GO was reduced to RGO. The phase angle also changed from 90° for PES-GO (capacitative behavior) to 0° for RGO coated fabrics (resistive behavior). In general an increase in the number of RGO layers produced an increase of the conductivity of the fabrics. EIS measurements in metal/sample/electrolyte configuration showed better electrocatalytic properties and faster diffusion rate for RGO specimens. Scanning electrochemical microscopy was employed to test the electroactivity of the different fabrics obtained. The sample coated with GO was not conductive since negative feedback was obtained. When GO was reduced to RGO the sample behaved like a conducting material since positive feedback was obtained. Approach curves indicated that the redox mediator had influence on the electrochemical response. The Fe(CN)63-/4- redox mediator produced a higher electrochemical response than Ru(NH3)63+/2+ one.

  16. Degradation of methylparathion in aqueous solution by electrochemical oxidation.

    PubMed

    Vlyssides, Apostolos; Barampouti, Elli Maria; Mai, Sofia; Arapoglou, Dimitris; Kotronarou, Anastasia

    2004-11-15

    The electrochemical degradation of methylparathion has been investigated by using Ti/Pt as anode, Stainless Steel 304 as cathode, and sodium chloride as electrolyte. The pesticide is rapidly degraded, but full mineralization is not observed. Degradation products have been monitored through gas chromatography and mass spectrometry, and the overall degradation process has been monitored through dissolved and particulate organic carbon, sulfur, and phosphorus measurements. Several intermediates have been identified, and oxalic, formic, and acetic acids as well as tetraphosphorus trisulfide have been recognized as final products of the degradation process. A proposed mechanism of the process is presented.

  17. Removal of the X-ray contrast media diatrizoate by electrochemical reduction and oxidation.

    PubMed

    Radjenovic, Jelena; Flexer, Victoria; Donose, Bogdan C; Sedlak, David L; Keller, Jurg

    2013-01-01

    Due to their resistance to biological wastewater treatment, iodinated X-ray contrast media (ICM) have been detected in municipal wastewater effluents at relatively high concentrations (i.e., up to 100 μg L(-1)), with hospitals serving as their main source. To provide a new approach for reducing the concentrations of ICMs in wastewater, electrochemical reduction at three-dimensional graphite felt and graphite felt doped with palladium nanoparticles was examined as a means for deiodination of the common ICM diatrizoate. The presence of palladium nanoparticles significantly enhanced the removal of diatrizoate and enabled its complete deiodination to 3,5-diacetamidobenzoic acid. When the system was employed in the treatment of hospital wastewater, diatrizoate was reduced, but the extent of electrochemical reduction decreased as a result of competing reactions with solutes in the matrix. Following electrochemical reduction of diatrizoate to 3,5-diacetamidobenzoic acid, electrochemical oxidation with boron-doped diamond (BDD) anodes was employed. 3,5-Diacetamidobenzoic acid disappeared from solution at a rate that was similar to that of diatrizoate, but it was more readily mineralized than the parent compound. When electrochemical reduction and oxidation were coupled in a three-compartment reactor operated in a continuous mode, complete deiodination of diatrizoate was achieved at an applied cathode potential of -1.7 V vs SHE, with the released iodide ions electrodialyzed in a central compartment with 80% efficiency. The resulting BDD anode potential (i.e., +3.4-3.5 V vs SHE) enabled efficient oxidation of the products of the reductive step. The presence of other anions (e.g., chloride) was likely responsible for a decrease in I(-) separation efficiency when hospital wastewater was treated. Reductive deiodination combined with oxidative degradation provides benefits over oxidative treatment methods because it does not produce stable iodinated intermediates. Nevertheless

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

    SciTech Connect

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

    2014-01-01

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

  19. Hollow CuO nanospheres uniformly anchored on porous Si nanowires: preparation and their potential use as electrochemical sensors

    NASA Astrophysics Data System (ADS)

    Guo, Zheng; Seol, Myeong-Lok; Kim, Moon-Seok; Ahn, Jae-Hyuk; Choi, Yang-Kyu; Liu, Jin-Huai; Huang, Xing-Jiu

    2012-11-01

    Hollow CuO nanospheres have been prepared via a reduction reaction of copper ions on porous Si nanowires combined with calcination in air and uniformly anchored on their surfaces. Scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) were employed to characterize and analyze as-synthesized samples. The results reveal that Si nanowires fabricated from heavily doped Si wafer are formed with a meso-porous structure by an Ag-assisted etching approach, and Cu nanoparticles are formed and uniformly decorated on the Si nanowires through a reaction of copper ions reduced by silicon. After annealing in air, Cu nanoparticles are in situ oxidized and transformed into CuO, leading to the formation of hollow nanospheres because of the Kirkendall effect. The diameter size of as-prepared CuO hollow spheres anchored on porous Si nanowires is mainly around 30 nm. Finally, in order to illuminate the advantages of this novel hybrid nanostructure of nanosized hollow spheres supported on porous nanowires, its electrochemical sensing performance to hydrazine as an example has been further investigated. The results confirm that it is a good potential application to detect hydrazine.Hollow CuO nanospheres have been prepared via a reduction reaction of copper ions on porous Si nanowires combined with calcination in air and uniformly anchored on their surfaces. Scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) were employed to characterize and analyze as-synthesized samples. The results reveal that Si nanowires fabricated from heavily doped Si wafer are formed with a meso-porous structure by an Ag-assisted etching approach, and Cu nanoparticles are formed and uniformly decorated on the Si nanowires through a reaction of copper ions reduced by silicon. After annealing in air, Cu nanoparticles are in situ oxidized and transformed into CuO, leading to the

  20. Boron-doped diamond electrodes for the electrochemical oxidation and cleavage of peptides.

    PubMed

    Roeser, Julien; Alting, Niels F A; Permentier, Hjalmar P; Bruins, Andries P; Bischoff, Rainer

    2013-07-16

    Electrochemical oxidation of peptides and proteins is traditionally performed on carbon-based electrodes. Adsorption caused by the affinity of hydrophobic and aromatic amino acids toward these surfaces leads to electrode fouling. We compared the performance of boron-doped diamond (BDD) and glassy carbon (GC) electrodes for the electrochemical oxidation and cleavage of peptides. An optimal working potential of 2000 mV was chosen to ensure oxidation of peptides on BDD by electron transfer processes only. Oxidation by electrogenerated OH radicals took place above 2500 mV on BDD, which is undesirable if cleavage of a peptide is to be achieved. BDD showed improved cleavage yield and reduced adsorption for a set of small peptides, some of which had been previously shown to undergo electrochemical cleavage C-terminal to tyrosine (Tyr) and tryptophan (Trp) on porous carbon electrodes. Repeated oxidation with BDD electrodes resulted in progressively lower conversion yields due to a change in surface termination. Cathodic pretreatment of BDD at a negative potential in an acidic environment successfully regenerated the electrode surface and allowed for repeatable reactions over extended periods of time. BDD electrodes are a promising alternative to GC electrodes in terms of reduced adsorption and fouling and the possibility to regenerate them for consistent high-yield electrochemical cleavage of peptides. The fact that OH-radicals can be produced by anodic oxidation of water at elevated positive potentials is an additional advantage as they allow another set of oxidative reactions in analogy to the Fenton reaction, thus widening the scope of electrochemistry in protein and peptide chemistry and analytics.

  1. Cerium-modified doped strontium titanate compositions for solid oxide fuel cell anodes and electrodes for other electrochemical devices

    SciTech Connect

    Marina, Olga A; Stevenson, Jeffry W

    2010-03-02

    The present invention provides novel compositions that find advantageous use in making electrodes for electrochemical cells and electrochemical devices such as solid oxide fuel cells, electrolyzers, sensors, pumps and the like, the compositions comprising cerium-modified doped strontium titanate. The invention also provides novel methods for making and using anode material compositions and solid oxide fuel cells and solid oxide fuel cell assemblies having anodes comprising the compositions.

  2. Copper-substituted perovskite compositions for solid oxide fuel cell cathodes and oxygen reduction electrodes in other electrochemical devices

    DOEpatents

    Rieke, Peter C [Pasco, WA; Coffey, Gregory W [Richland, WA; Pederson, Larry R [Kennewick, WA; Marina, Olga A [Richland, WA; Hardy, John S [Richland, WA; Singh, Prabhaker [Richland, WA; Thomsen, Edwin C [Richland, WA

    2010-07-20

    The present invention provides novel compositions that find advantageous use in making electrodes for electrochemical cells. Also provided are electrochemical devices that include active oxygen reduction electrodes, such as solid oxide fuel cells, sensors, pumps and the like. The compositions comprises a copper-substituted ferrite perovskite material. The invention also provides novel methods for making and using the electrode compositions and solid oxide fuel cells and solid oxide fuel cell assemblies having cathodes comprising the compositions.

  3. Cerium-modified doped strontium titanate compositions for solid oxide fuel cell anodes and electrodes for other electrochemical devices

    DOEpatents

    Marina, Olga A [Richland, WA; Stevenson, Jeffry W [Richland, WA

    2010-11-23

    The present invention provides novel compositions that find advantageous use in making electrodes for electrochemical cells and electrochemical devices such as solid oxide fuel cells, electrolyzers, sensors, pumps and the like, the compositions comprising cerium-modified doped strontium titanate. The invention also provides novel methods for making and using anode material compositions and solid oxide fuel cells and solid oxide fuel cell assemblies having anodes comprising the compositions.

  4. Metal Oxide Materials and Collector Efficiency in Electrochemical Supercapacitors

    DTIC Science & Technology

    2010-12-01

    composites can be deposited sponta- neously on carbon substrates, (iv) thin film mixed oxide systems showed promising power densities, especially in...Materials Characterization . . . . . . . . . . . . . . . . . . . . . 18 5 Thin film mixed oxide electrodes...titanium substrate. . . . . . . . . . . . . . . . . . . 26 Figure 17: X-ray diffraction patterns for RuxMn1-xO2 thin film coated titanium substrates The

  5. Simple room-temperature preparation of high-yield large-area graphene oxide.

    PubMed

    Huang, N M; Lim, H N; Chia, C H; Yarmo, M A; Muhamad, M R

    2011-01-01

    Graphene has attracted much attention from researchers due to its interesting mechanical, electrochemical, and electronic properties. It has many potential applications such as polymer filler, sensor, energy conversion, and energy storage devices. Graphene-based nanocomposites are under an intense spotlight amongst researchers. A large amount of graphene is required for preparation of such samples. Lately, graphene-based materials have been the target for fundamental life science investigations. Despite graphene being a much sought-after raw material, the drawbacks in the preparation of graphene are that it is a challenge amongst researchers to produce this material in a scalable quantity and that there is a concern about its safety. Thus, a simple and efficient method for the preparation of graphene oxide (GO) is greatly desired to address these problems. In this work, one-pot chemical oxidation of graphite was carried out at room temperature for the preparation of large-area GO with ~100% conversion. This high-conversion preparation of large-area GO was achieved using a simplified Hummer's method from large graphite flakes (an average flake size of 500 μm). It was found that a high degree of oxidation of graphite could be realized by stirring graphite in a mixture of acids and potassium permanganate, resulting in GO with large lateral dimension and area, which could reach up to 120 μm and ~8000 μm(2), respectively. The simplified Hummer's method provides a facile approach for the preparation of large-area GO.

  6. Vanadium oxide nanodisks: Synthesis, characterization, and electrochemical properties

    SciTech Connect

    Ren, Ling; Cao, Minhua; Shi, Shufeng; Hu, Changwen

    2012-01-15

    Highlights: Black-Right-Pointing-Pointer Highly crystallined VO{sub 1.6}{center_dot}H{sub 2}O nanodisks have been synthesized by using a novel solid-solution-solid growth process. Black-Right-Pointing-Pointer The nanodisks are assembled from nanoparticles. Black-Right-Pointing-Pointer PEG-4000 plays an important role for the formation of the nanodisks. Black-Right-Pointing-Pointer The as-synthesized nanodisks exhibit good electrochemical behavior. -- Abstract: Highly crystallined VO{sub 1.6}{center_dot}H{sub 2}O nanodisks assembled from nanoparticles have been successfully fabricated under hydrothermal conditions by using bulk V{sub 2}O{sub 5} and Na{sub 2}S{sub 2}O{sub 3} as the starting materials in the presence of surfactant polyethylene glycol 4000 (PEG-4000). The nanodisks have a diameter of 200 nm and thickness of 40 nm. Hollow nanodisks are occasionally observed, which is similar to Chinese ancient copper coins. The formation of nanodisks can be ascribed to a novel solid-solution-solid growth mechanism. Compared with other methods, the solid state transformation method is simple and economic. In addition, the nanodisks exhibit good electrochemical behavior and promising to be used in lithium-ion battery.

  7. Formulation and method for preparing gels comprising hydrous hafnium oxide

    DOEpatents

    Collins, Jack L; Hunt, Rodney D; Montgomery, Frederick C

    2013-08-06

    Formulations useful for preparing hydrous hafnium oxide gels contain a metal salt including hafnium, an acid, an organic base, and a complexing agent. Methods for preparing gels containing hydrous hafnium oxide include heating a formulation to a temperature sufficient to induce gel formation, where the formulation contains a metal salt including hafnium, an acid, an organic base, and a complexing agent.

  8. Formulation and method for preparing gels comprising hydrous aluminum oxide

    DOEpatents

    Collins, Jack L.

    2014-06-17

    Formulations useful for preparing hydrous aluminum oxide gels contain a metal salt including aluminum, an organic base, and a complexing agent. Methods for preparing gels containing hydrous aluminum oxide include heating a formulation to a temperature sufficient to induce gel formation, where the formulation contains a metal salt including aluminum, an organic base, and a complexing agent.

  9. Formulation and method for preparing gels comprising hydrous cerium oxide

    SciTech Connect

    Collins, Jack L; Chi, Anthony

    2013-05-07

    Formulations useful for preparing hydrous cerium oxide gels contain a metal salt including cerium, an organic base, and a complexing agent. Methods for preparing gels containing hydrous cerium oxide include heating a formulation to a temperature sufficient to induce gel formation, where the formulation contains a metal salt including cerium, an organic base, and a complexing agent.

  10. Electrochemical analysis of transparent oxide-less photovoltaic cell with perforation patterned metal substrate

    NASA Astrophysics Data System (ADS)

    Kim, Myoung; You, In-Kyu; Lee, Kyoung-Won; Lee, In-Hwan; Yun, Ho-Gyeong

    2013-05-01

    In terms of electrochemical behaviour, a transparent conductive oxide (TCO)-less dye-sensitized solar cell (DSSC) with two metal foils was compared with those of a metal foil-based DSSC with a TCO-coated substrate. By virtue of electrochemical impedance spectroscopy, intensity modulated photocurrent spectroscopy, intensity modulated photovoltage spectroscopy, open-circuit voltage decay, and photocurrent transient measurements, it was clearly confirmed that the limited performance of the TCO-less DSSC was caused by the restricted transport of ion species in the electrolyte due to the perforation patterned metal foil.

  11. Direct correlation of electrochemical behaviors with anti-thrombogenicity of semiconducting titanium oxide films.

    PubMed

    Wan, Guojiang; Lv, Bo; Jin, Guoshou; Maitz, Manfred F; Zhou, Jianzhang; Huang, Nan

    2014-01-01

    Biomaterials-associated thrombosis is dependent critically upon electrochemical response of fibrinogen on material surface. The relationship between the response and anti-thrombogenicity of biomaterials is not well-established. Titanium oxide appears to have good anti-thrombogenicity and little is known about its underlying essential chemistry. We correlate their anti-thrombogenicity directly to electrochemical behaviors in fibrinogen containing buffer solution. High degree of inherent n-type doping was noted to contribute the impedance preventing charge transfer from fibrinogen into film (namely its activation) and consequently reduced degree of anti-thrombogenicity. The impedance was the result of high donor carrier density as well as negative flat band potential.

  12. Ammonium nitrogen removal from wastewater with a three-dimensional electrochemical oxidation system.

    PubMed

    Ding, Jing; Zhao, Qing-Liang; Wei, Liang-Liang; Chen, Yang; Shu, Xin

    2013-01-01

    Ammonium-containing wastewater could cause the promotion of eutrophication and a hindrance to the disinfection of water supplies. In this study, the feasibility of removing low-concentration ammonium nitrogen from synthetic and real wastewater by electrochemical oxidation was investigated. Using laboratory-scale electrochemical systems, the effects of chloride concentration, current density, anode materials, cathode materials, electrode gap, initial ammonium concentration and three-dimensional particles on the removal of ammonium nitrogen and current efficiency (CE) were evaluated. Ammonium nitrogen removal was mainly dependent upon anode materials and current density. The performance of two- and three-dimensional electrochemical oxidation systems was comparatively discussed. Both particle electrodes could enhance ammonium nitrogen removal and increase CE. However, the mechanism of the process seemed to be different. Moreover, the interaction of zeolites adsorption and electrochemical oxidation on the anode in a three-dimensional system could favor the regeneration of zeolites. Surface morphology of the used Ru-Ir-Sn/Ti anode revealed its longer working life of electrocatalysis. The result of ammonium degradation for a real wastewater treatment plant effluent showed the degradation rates in a three-dimensional system increased by 1.4 times those in a two-dimensional system.

  13. Electron transfer of Pseudomonas aeruginosa CP1 in electrochemical reduction of nitric oxide.

    PubMed

    Zhou, Shaofeng; Huang, Shaobin; He, Jiaxin; Li, Han; Zhang, Yongqing

    2016-10-01

    This study reports catalytic electro-chemical reduction of nitric oxide (NO) enhanced by Pseudomonas aeruginosa strain CP1. The current generated in the presence of bacteria was 4.36times that in the absence of the bacteria. The strain was able to catalyze electro-chemical reduction of NO via indirect electron transfer with an electrode, revealed by a series of cyclic voltammetry experiments. Soluble electron shuttles secreted into solution by live bacteria were responsible for the catalytic effects. The enhancement of NO reduction was also confirmed by detection of nitrous oxide; the level of this intermediate was 46.4% higher in the presence of bacteria than in controls, illustrated that the electron transfer pathway did not directly reduce nitric oxide to N2. The findings of this study may offer a new model for bioelectrochemical research in the field of NO removal by biocatalysts.

  14. Electrochemical and theoretical characterization of the electro-oxidation of dimethoxycurcumin

    NASA Astrophysics Data System (ADS)

    Arrue, Lily; Barra, Tomas; Camarada, María Belén; Zarate, Ximena; Schott, Eduardo

    2017-06-01

    Dimethoxycurcumin (DMC) ((1E,6E)-1-(3,4-dimethoxycyclohexyl)-7-(3,4-dimethoxyphenyl) hepta-1,6- diene-3,5-dione) is a natural polyphenolic compound that appears together with curcumin in turmeric. Both molecules have wide range biological activities as antioxidant, anti-inflammatory and anti-carcinogenic agent. To evaluate the oxidation process and kinetics for DMC, the rate constant, electron transfer and diffusion coefficients for the electrochemical oxidation were determined. Therefore, its electrochemical behavior over a platinum electrode in anhydrous media was investigated. Furthermore, DFT calculations were performed to give a rational explanation to the obtained results. All the results support the fact that the central sbnd CH2sbnd group is the most reactive against an oxidation process.

  15. Recent advances in nanostructured Nb-based oxides for electrochemical energy storage

    NASA Astrophysics Data System (ADS)

    Yan, Litao; Rui, Xianhong; Chen, Gen; Xu, Weichuan; Zou, Guifu; Luo, Hongmei

    2016-04-01

    For the past five years, nanostructured niobium-based oxides have emerged as one of the most prominent materials for batteries, supercapacitors, and fuel cell technologies, for instance, TiNb2O7 as an anode for lithium-ion batteries (LIBs), Nb2O5 as an electrode for supercapacitors (SCs), and niobium-based oxides as chemically stable electrochemical supports for fuel cells. Their high potential window can prevent the formation of lithium dendrites, and their rich redox chemistry (Nb5+/Nb4+, Nb4+/Nb3+) makes them very promising electrode materials. Their unique chemical stability under acid conditions is favorable for practical fuel-cell operation. In this review, we summarized recent progress made concerning the use of niobium-based oxides as electrodes for batteries (LIBs, sodium-ion batteries (SIBs), and vanadium redox flow batteries (VRBs)), SCs, and fuel cell applications. Moreover, crystal structures, charge storage mechanisms in different crystal structures, and electrochemical performances in terms of the specific capacitance/capacity, rate capability, and cycling stability of niobium-based oxides are discussed. Insights into the future research and development of niobium-based oxide compounds for next-generation electrochemical devices are also presented. We believe that this review will be beneficial for research scientists and graduate students who are searching for promising electrode materials for batteries, SCs, and fuel cells.

  16. Electrochemical treatment of aqueous wastes containing pyrogallol by BDD-anodic oxidation.

    PubMed

    Nasr, Bensalah; Hsen, Trabelsi; Abdellatif, Gadri

    2009-01-01

    In this work, the electrochemical oxidation of pyrogallol (1,2,3-trihydroxybenzene) on boron-doped diamond anodes has been studied. The voltammetric results showed that pyrogallol oxidation takes place in the same potential region as that of phenol where the supporting electrolyte is stable. Synthetic wastewaters containing pyrogallol have been treated in a bench-scale electrolysis plant. This plant operates in a discontinuous mode by recirculating the waste continuously through a single-chamber electrochemical flow cell. The complete mineralization of pyrogallol and the electro-generated pollutants is obtained in the electrolytic device. HPLC analyses show the formation of carboxylic acids as the main intermediates. The efficiency of the electrochemical process was found to depend mainly on the pollutant concentration present in the waste and on the applied current density. The high efficiency of this technology can be explained in terms of the direct electro-oxidation at the BDD surface and the oxidation carried out by hydroxyl radicals and other electro-generated oxidants.

  17. Recent advances in nanostructured Nb-based oxides for electrochemical energy storage.

    PubMed

    Yan, Litao; Rui, Xianhong; Chen, Gen; Xu, Weichuan; Zou, Guifu; Luo, Hongmei

    2016-04-28

    For the past five years, nanostructured niobium-based oxides have emerged as one of the most prominent materials for batteries, supercapacitors, and fuel cell technologies, for instance, TiNb2O7 as an anode for lithium-ion batteries (LIBs), Nb2O5 as an electrode for supercapacitors (SCs), and niobium-based oxides as chemically stable electrochemical supports for fuel cells. Their high potential window can prevent the formation of lithium dendrites, and their rich redox chemistry (Nb(5+)/Nb(4+), Nb(4+)/Nb(3+)) makes them very promising electrode materials. Their unique chemical stability under acid conditions is favorable for practical fuel-cell operation. In this review, we summarized recent progress made concerning the use of niobium-based oxides as electrodes for batteries (LIBs, sodium-ion batteries (SIBs), and vanadium redox flow batteries (VRBs)), SCs, and fuel cell applications. Moreover, crystal structures, charge storage mechanisms in different crystal structures, and electrochemical performances in terms of the specific capacitance/capacity, rate capability, and cycling stability of niobium-based oxides are discussed. Insights into the future research and development of niobium-based oxide compounds for next-generation electrochemical devices are also presented. We believe that this review will be beneficial for research scientists and graduate students who are searching for promising electrode materials for batteries, SCs, and fuel cells.

  18. Structure and Optical Features of Micro/Nanosized Carbon Forms Prepared by Electrochemical Exfoliation

    NASA Astrophysics Data System (ADS)

    Nedilko, Sergii G.; Revo, Sergiy; Chornii, Vitalii; Scherbatskyi, Vasyl; Ivanenko, Kateryna; Nedielko, Maksym; Sementsov, Yurii; Skoryk, Mykola; Nikolenko, Andrii; Strelchuk, Victor

    2017-01-01

    Micro/nanosized carbon materials were prepared by electrochemical exfoliation method in the forms of the colloids and thin films. Scanning electronic microscopy, optical and luminescent microscopy, and Raman scattering and luminescent spectroscopy were applied for characterization of materials. The wide photoluminescence band in the visible spectral region was observed for each of the samples. The shape of the photoluminescence band depends on excitation wavelength and on the size of the particles. At least two components with maxima at 580 and 710 nm can be distinguished in the photoluminescence spectra. The relations between the photoluminescence properties and morphology of the samples have been described and discussed.

  19. Performance of flexible capacitors based on polypyrrole/carbon fiber electrochemically prepared from various phosphate electrolytes

    NASA Astrophysics Data System (ADS)

    Yuan, Wei; Han, Gaoyi; Chang, Yunzhen; Li, Miaoyu; Xiao, Yaoming; Zhou, Haihan; Zhang, Ying; Li, Yanping

    2016-11-01

    In order to investigate the influence of electrolytes in electro-deposition solution on the capacitive properties of polypyrrole (PPy), we have chosen phosphoric acid, phosphate, hydrogen phosphate and dihydrogen phosphate as electrolyte in deposition solution respectively and electrochemically deposited PPy on carbon fibers (CFs) via galvanostatic method. The morphologies of the PPy/CFs samples have been characterized by scanning electron microscope. The specific capacitance of PPy/CFs samples has been evaluated in different electrolytes through three-electrode test system. The assembled flexible capacitors by using PPy/CFs as electrodes and H3PO4/polyvinyl alcohol as gel electrolyte have been systematically measured by cyclic voltammetry, galvanostatic charge/discharge and electrochemical impedance spectroscopy. The results show that the electrochemical capacitors based on PPy/CFs prepared from deposition solution containing NaH2PO4·2H2O electrolyte exhibit higher specific capacitance, flexibility and excellent stability (retaining 96.8% of initial capacitance after 13,000 cycles), and that three cells connected in series can power a light-emitting diode.

  20. Modified cermet fuel electrodes for solid oxide electrochemical cells

    DOEpatents

    Ruka, Roswell J.; Spengler, Charles J.

    1991-01-01

    An exterior porous electrode (10), bonded to a solid oxygen ion conducting electrolyte (13) which is in contact with an interior electrode (14), contains coarse metal particles (12) of nickel and/or cobalt, having diameters from 3 micrometers to 35 micrometers, where the coarse particles are coated with a separate, porous, multiphase layer (17) containing fine metal particles of nickel and/or cobalt (18), having diameters from 0.05 micrometers to 1.75 micrometers and conductive oxide (19) selected from cerium oxide, doped cerium oxide, strontium titanate, doped strontium titanate and mixtures thereof.

  1. Theoretical investigation of the activity of cobalt oxides for the electrochemical oxidation of water.

    PubMed

    Bajdich, Michal; García-Mota, Mónica; Vojvodic, Aleksandra; Nørskov, Jens K; Bell, Alexis T

    2013-09-11

    The presence of layered cobalt oxides has been identified experimentally in Co-based anodes under oxygen-evolving conditions. In this work, we report the results of theoretical investigations of the relative stability of layered and spinel bulk phases of Co oxides, as well as the stability of selected surfaces as a function of applied potential and pH. We then study the oxygen evolution reaction (OER) on these surfaces and obtain activity trends at experimentally relevant electro-chemical conditions. Our calculated volume Pourbaix diagram shows that β-CoOOH is the active phase where the OER occurs in alkaline media. We calculate relative surface stabilities and adsorbate coverages of the most stable low-index surfaces of β-CoOOH: (0001), (0112), and (1014). We find that at low applied potentials, the (1014) surface is the most stable, while the (0112) surface is the more stable at higher potentials. Next, we compare the theoretical overpotentials for all three surfaces and find that the (1014) surface is the most active one as characterized by an overpotential of η = 0.48 V. The high activity of the (1014) surface can be attributed to the observation that the resting state of Co in the active site is Co(3+) during the OER, whereas Co is in the Co(4+) state in the less active surfaces. Lastly, we demonstrate that the overpotential of the (1014) surface can be lowered further by surface substitution of Co by Ni. This finding could explain the experimentally observed enhancement in the OER activity of Ni(y)Co(1-y)O(x) thin films with increasing Ni content. All energetics in this work were obtained from density functional theory using the Hubbard-U correction.

  2. Coating of tips for electrochemical scanning tunneling microscopy by means of silicon, magnesium, and tungsten oxides.

    PubMed

    Salerno, Marco

    2010-09-01

    Different combinations of metal tips and oxide coatings have been tested for possible operation in electrochemical scanning tunneling microscopy. Silicon and magnesium oxides have been thermally evaporated onto gold and platinum-iridium tips, respectively. Two different thickness values have been explored for both materials, namely, 40 and 120 nm for silicon oxide and 20 and 60 nm for magnesium oxide. Alternatively, tungsten oxide has been grown on tungsten tips via electrochemical anodization. In the latter case, to seek optimal results we have varied the pH of the anodizing electrolyte between one and four. The oxide coated tips have been first inspected by means of scanning electron microscopy equipped with microanalysis to determine the morphological results of the coating. Second, the coated tips have been electrically characterized ex situ for stability in time by means of cyclic voltammetry in 1 M aqueous KCl supporting electrolyte, both bare and supplemented with K(3)[Fe(CN)(6)] complex at 10 mM concentration in milliQ water as an analyte. Only the tungsten oxide coated tungsten tips have shown stable electrical behavior in the electrolyte. For these tips, the uncoated metal area has been estimated from the electrical current levels, and they have been successfully tested by imaging a gold grating in situ, which provided stable results for several hours. The successful tungsten oxide coating obtained at pH=4 has been assigned to the WO(3) form.

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

    NASA Astrophysics Data System (ADS)

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

    2017-05-01

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

  4. Method for preparing hydrous zirconium oxide gels and spherules

    DOEpatents

    Collins, Jack L.

    2003-08-05

    Methods for preparing hydrous zirconium oxide spherules, hydrous zirconium oxide gels such as gel slabs, films, capillary and electrophoresis gels, zirconium monohydrogen phosphate spherules, hydrous zirconium oxide spherules having suspendable particles homogeneously embedded within to form a composite sorbent, zirconium monohydrogen phosphate spherules having suspendable particles of at least one different sorbent homogeneously embedded within to form a composite sorbent having a desired crystallinity, zirconium oxide spherules having suspendable particles homogeneously embedded within to form a composite, hydrous zirconium oxide fiber materials, zirconium oxide fiber materials, hydrous zirconium oxide fiber materials having suspendable particles homogeneously embedded within to form a composite, zirconium oxide fiber materials having suspendable particles homogeneously embedded within to form a composite and spherules of barium zirconate. The hydrous zirconium oxide spherules and gel forms prepared by the gel-sphere, internal gelation process are useful as inorganic ion exchangers, catalysts, getters and ceramics.

  5. Advanced treatment of biologically pretreated coking wastewater by electrochemical oxidation using boron-doped diamond electrodes.

    PubMed

    Zhu, Xiuping; Ni, Jinren; Lai, Peng

    2009-09-01

    Electrochemical oxidation is a promising technology to treatment of bio-refractory wastewater. Coking wastewater contains high concentration of refractory and toxic compounds and the water quality usually cannot meet the discharge standards after conventional biological treatment processes. This paper initially investigated the electrochemical oxidation using boron-doped diamond (BDD) anode for advanced treatment of coking wastewater. Under the experimental conditions (current density 20-60mAcm(-2), pH 3-11, and temperature 20-60 degrees C) using BDD anode, complete mineralization of organic pollutants was almost achieved, and surplus ammonia-nitrogen (NH(3)-N) was further removed thoroughly when pH was not adjusted or at alkaline value. Moreover, the TOC and NH(3)-N removal rates in BDD anode cell were much greater than those in other common anode systems such as SnO(2) and PbO(2) anodes cells. Given the same target to meet the National Discharge Standard of China, the energy consumption of 64kWhkgCOD(-1) observed in BDD anode system was only about 60% as much as those observed in SnO(2) and PbO(2) anode systems. Further investigation revealed that, in BDD anode cell, organic pollutants were mainly degraded by reaction with free hydroxyl radicals and electrogenerated oxidants (S(2)O(8)(2-), H(2)O(2), and other oxidants) played a less important role, while direct electrochemical oxidation and indirect electrochemical oxidation mediated by active chlorine can be negligible. These results showed great potential of BDD anode system in engineering application as a final treatment of coking wastewater.

  6. Tin Oxide Nanorod Array-Based Electrochemical Hydrogen Peroxide Biosensor

    PubMed Central

    2010-01-01

    SnO2 nanorod array grown directly on alloy substrate has been employed as the working electrode of H2O2 biosensor. Single-crystalline SnO2 nanorods provide not only low isoelectric point and enough void spaces for facile horseradish peroxidase (HRP) immobilization but also numerous conductive channels for electron transport to and from current collector; thus, leading to direct electrochemistry of HRP. The nanorod array-based biosensor demonstrates high H2O2 sensing performance in terms of excellent sensitivity (379 μA mM−1 cm−2), low detection limit (0.2 μM) and high selectivity with the apparent Michaelis–Menten constant estimated to be as small as 33.9 μM. Our work further demonstrates the advantages of ordered array architecture in electrochemical device application and sheds light on the construction of other high-performance enzymatic biosensors. PMID:20596358

  7. Tin Oxide Nanorod Array-Based Electrochemical Hydrogen Peroxide Biosensor

    NASA Astrophysics Data System (ADS)

    Liu, Jinping; Li, Yuanyuan; Huang, Xintang; Zhu, Zhihong

    2010-07-01

    SnO2 nanorod array grown directly on alloy substrate has been employed as the working electrode of H2O2 biosensor. Single-crystalline SnO2 nanorods provide not only low isoelectric point and enough void spaces for facile horseradish peroxidase (HRP) immobilization but also numerous conductive channels for electron transport to and from current collector; thus, leading to direct electrochemistry of HRP. The nanorod array-based biosensor demonstrates high H2O2 sensing performance in terms of excellent sensitivity (379 μA mM-1 cm-2), low detection limit (0.2 μM) and high selectivity with the apparent Michaelis-Menten constant estimated to be as small as 33.9 μM. Our work further demonstrates the advantages of ordered array architecture in electrochemical device application and sheds light on the construction of other high-performance enzymatic biosensors.

  8. Non-covalent functionalization of graphene oxide by polyindole and subsequent incorporation of Ag nanoparticles for electrochemical applications

    NASA Astrophysics Data System (ADS)

    Dubey, Prashant; Kumar, Ashish; Prakash, Rajiv

    2015-11-01

    Reduced graphene oxide (r-GO) sheets have been modified by polyindole (PIn) via in situ chemical oxidation method to obtain stable dispersion in water and furthermore incorporation of Ag nanoparticles (Ag NPs); the resulting Ag NPs/PIn-r-GO nanocomposite is demonstrated for electrochemical applications. Ag NPs/r-GO and PIn/GO nanocomposites have also been prepared for its comparative study with Ag NPs/PIn-r-GO. Non-covalent functionalization of GO by PIn polymer leads to PIn-GO dispersion, which is stable for several months without any precipitation. This dispersed solution is used for formation of Ag NPs/PIn-r-GO nanocomposite. Various experimental tools like UV-vis, FTIR and TEM have been used to characterize as-synthesized materials. Thereafter electrochemical performance of as-synthesized nanocomposites have been compared for their charge capacitive behaviour (without its poisoning compared to Ag NPs/r-GO) which leads to be an excellent candidate for the possible applications such as electrocatalysis, charge storage devices, etc. We observed that Ag NPs/PIn-r-GO nanocomposite exhibits better processability and electroactivity as electrode material in comparison to Ag NPs/r-GO and PIn/GO nanocomposites due to synergistic effect of individual components.

  9. Platinum/mesoporous WO3 as a carbon-free electrocatalyst with enhanced electrochemical activity for methanol oxidation.

    PubMed

    Cui, Xiangzhi; Shi, Jianlin; Chen, Hangrong; Zhang, Lingxia; Guo, Limin; Gao, Jianhua; Li, Jingbo

    2008-09-25

    A new type of carbon-free electrode catalyst, Pt/mesoporous WO3 composite, has been prepared and its electrochemical activity for methanol oxidation has been investigated. The mesoporous tungsten trioxide support was synthesized by a replicating route and the mesoporous composties with Pt loaded were characterized by using X-ray diffraction (XRD), nitrogen sorption, field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy (EDS) techniques. Cyclic voltammetry (CV), line scan voltammetry (LSV) and chronoamperometry (CA) were adopted to characterize the electrochemical activities of the composites. The mesoporous WO3 showed high surface area, ordered pore structure, and nanosized wall thickness of about 6-7 nm. When a certain amount of Pt nanoparticles were dispersed in the pore structure of mesoporous WO3, the resultant mesostructured Pt/WO3 composites exhibit high electro-catalytic activity toward methanol oxidation. The overall electro-catalytic activities of 20 wt % Pt/WO3 composites are significantly higher than that of commercial 20 wt % Pt/C catalyst and are comparable to the 20 wt % PtRu/C catalyst in the potential region of 0.5-0.7 V. The enhanced electro-catalytic activity is attributed to be resulted from the assistant catalytic effect and the mesoporous structure of WO3 supports.

  10. Electrochemical characteristics of the reduced graphene oxide/carbon nanotube/polypyrrole composites for aqueous asymmetric supercapacitors

    NASA Astrophysics Data System (ADS)

    Peng, Yu-Jung; Wu, Tzu-Ho; Hsu, Chun-Tsung; Li, Shin-Ming; Chen, Ming-Guan; Hu, Chi-Chang

    2014-12-01

    Polypyrrole (PPy) has been polymerized onto reduced graphene oxide/carbon nanotube (rGO/CNT) to form an rGO/CNT/PPy composite using the chemical oxidation method. The electrochemical characteristics of the above composite in various aqueous electrolytes are systematically compared for the asymmetric supercapacitor application. The electrochemical characteristics of rGO/CNT/PPy in the electrolytes containing K+ show improved reversibility and higher stability. Introducing XC-72 in preparing the electrode has been found to enhance the specific capacitance and the cycle stability of rGO/CNT/PPy. The charge storage stability of rGO/CNT/PPy + XC-72 in various potential windows has been evaluated through the potential bias stress test. An asymmetric supercapacitor (ASC) with a positive electrode of Mn3O4 and a negative electrode of rGO/CNT/PPy + XC-72 is successfully demonstrated, which shows specific energy and power of 14. Wh kg-1 and 6.62 kW kg-1 with a cell voltage of 1.6 V. This ASC with a cell voltage of 1.6 V shows excellent charge-discharge cycle stability and ideal capacitive behavior in NaNO3 even after the application of 3250 charge-discharge cycles.

  11. Alkane Oxidation by a Particulate Preparation from Candida

    PubMed Central

    Liu, Chao-Min; Johnson, Marvin J.

    1971-01-01

    The oxidation of decane by a cell-free particulate preparation from Candida intermedia was studied. Decane is oxidized to decanoate via decanol and decanaldehyde. Oxidation of decane to decanol requires molecular oxygen. Decanol is oxidized to decanaldehyde by a nicotinamide adenine dinucleotide-linked dehydrogenase differing greatly in specificity from ordinary yeast alcohol dehydrogenase. Decanaldehyde is oxidized to decanoate by a nicotinamide adenine dinucleotide-linked dehydrogenase that oxidizes long-chain aldehydes but not short-chain aldehydes. The enzymes that oxidize decane, decanol, and decanaldehyde are all induced when decane is present in the medium. These enzymes are apparently located in the cell membrane. PMID:4326743

  12. Ruthenium Oxide Electrochemical Super Capacitor Optimization for Pulse Power Applications

    NASA Technical Reports Server (NTRS)

    Merryman, Stephen A.; Chen, Zheng

    2000-01-01

    Electrical actuator systems are being pursued as alternatives to hydraulic systems to reduce maintenance time, weight and costs while increasing reliability. Additionally, safety and environmental hazards associated with the hydraulic fluids can be eliminated. For most actuation systems, the actuation process is typically pulsed with high peak power requirements but with relatively modest average power levels. The power-time requirements for electrical actuators are characteristic of pulsed power technologies where the source can be sized for the average power levels while providing the capability to achieve the peak requirements. Among the options for the power source are battery systems, capacitor systems or battery-capacitor hybrid systems. Battery technologies are energy dense but deficient in power density; capacitor technologies are power dense but limited by energy density. The battery-capacitor hybrid system uses the battery to supply the average power and the capacitor to meet the peak demands. It has been demonstrated in previous work that the hybrid electrical power source can potentially provide a weight savings of approximately 59% over a battery-only source. Electrochemical capacitors have many properties that make them well-suited for electrical actuator applications. They have the highest demonstrated energy density for capacitive storage (up to 100 J/g), have power densities much greater than most battery technologies (greater than 30kW/kg), are capable of greater than one million charge-discharge cycles, can be charged at extremely high rates, and have non-explosive failure modes. Thus, electrochemical capacitors exhibit a combination of desirable battery and capacitor characteristics.

  13. Preparation of nickel nanowire arrays electrode for urea electro-oxidation in alkaline medium

    NASA Astrophysics Data System (ADS)

    Guo, Fen; Ye, Ke; Cheng, Kui; Wang, Guiling; Cao, Dianxue

    2015-03-01

    Fully metallic nickel nanowire arrays (NWAs) electrode is prepared by electrodepositing nickel within the pores and over-plating on the surface of polycarbonate template (PCT) with subsequent dissolution of the template in dichloromethane. The as-prepared electrode is characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Urea electro-oxidation reaction in KOH solution on the nickel NWAs electrode is investigated by cyclic voltammetry (CV), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) tests. The results show that the nickel NWAs electrode achieves an onset oxidation potential of 0.25 V (vs. Ag/AgCl) and a peak current density of 160 mA cm-2 in 5 mol L-1 KOH and 0.33 mol L-1 urea accompanied with considerable stability.

  14. Immobilization of methylviologen between well-ordered multilayers of manganese oxide during their electrochemical assembly.

    PubMed

    Nakayama, Masaharu; Hoyashita, Ryo; Komatsu, Hiroyuki; Muneyama, Etsuhiro; Shoda, Kaoru; Kunishige, Atsuhiro

    2007-03-13

    Methylviologen dications (MV2+) were immobilized between layers of manganese oxide during their electrochemical assembly by an anodic route in a homogeneous aqueous Mn2+ solution. This approach yielded a well-ordered multilayer film on a platinum substrate as a result of dense packing of planar MV2+ molecules to stabilize the layered framework. A grazing angle in-plane X-ray diffraction study revealed that the manganese oxide sheets and the molecular planes of inserted MV2+ ions are oriented parallel to the electrode surface. Cyclic voltammetry of the product film indicated an electron transfer from the underlying Pt substrate to inserted methylviologen ions through the manganese oxide sheets.

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

    NASA Astrophysics Data System (ADS)

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

    2017-02-01

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

  16. Enhancing electrochemical detection on graphene oxide-CNT nanostructured electrodes using magneto-nanobioprobes

    PubMed Central

    Sharma, Priyanka; Bhalla, Vijayender; Dravid, Vinayak; Shekhawat, Gajendera; Jinsong-Wu, J W; Prasad, E. Senthil; Suri, C. Raman

    2012-01-01

    Graphene and related materials have come to the forefront of research in electrochemical sensors during recent years due to the promising properties of these nanomaterials. Further applications of these nanomaterials have been hampered by insufficient sensitivity offered by these nanohybrids for the type of molecules requiring lower detection ranges. Here, we report a signal amplification strategy based on magneto-electrochemical immunoassay which combines the advantages of carbon nanotube and reduced graphene oxide together with electrochemical bursting of magnetic nanoparticles into a large number of metal ions. Sensitive detection was achieved by precisely designing the nanohybrid and correlating the available metal ions with analyte concentration. We confirmed the ultrahigh sensitivity of this method for a new generation herbicide diuron and its analogues up to sub-picomolar concentration in standard water samples. The novel immune-detection platform showed the excellent potential applicability in rapid and sensitive screening of environmental pollutants or toxins in samples. PMID:23166860

  17. Preparation and characterization of amine functionalized graphene oxide with water soluble quantum dots for sensing material

    NASA Astrophysics Data System (ADS)

    Zaid, Mohd Hazani Mat; Abdullah, Jaafar

    2017-09-01

    Nanocomposite material has been prepared comprises of amine functionalized graphene oxide (NH2-GO) incorporation with water solube CdS Quantum dots nanoparticle to form a new composite material (NH2-GO/QDs). This composite mixture shows highly homogenous without precipitation and have been characterize by using Raman, Fourier transform infrared spectroscopy (FTIR) and the scan electron microscopy (SEM-EDX). Kinetic investigation based on DNA hybridization by cyclic voltammetry shows modified electrode able to achieve high hybridization rate can be used as electrochemical biosensor platform.

  18. A novel preparation method of Sn-modified Pt nanoparticles and application for methanol oxidation

    NASA Astrophysics Data System (ADS)

    Du, Yongling; Su, Biquan; Zhang, Nuo; Wang, Chunming

    2008-12-01

    With polystyrene latex spheres self-assembled on ITO glass as templates, highly ordered two-dimensional (2D) Pt nanoparticles (PtNPs) were prepared by electrochemical deposition. The morphology and element composition of PtNPs were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The electrocatalytic properties of PtNPs/ITO and Sn underpotential deposition (UPD) modified PtNPs/ITO for methanol oxidation has been investigated by cyclic voltammetry (CV) and chronoamperometry (CA). The excellent electrocatalytic activity can be observed for these catalytic systems.

  19. [Degradation of aniline by a dual-electrode electrochemical oxidation process].

    PubMed

    Cen, Shi-Hong; Song, Xiao-Yan; Chu, Yan-Yang

    2011-08-01

    The efficiency and the mechanism of aniline degradation by an electrochemical oxidation process using a Ti/SnO2-Sb2O5 electrode as the anode and a graphite electrode as the cathode, were studied in two aqueous electrolytes with/without Fe2+. The results showed that the reasonable anodic potential was about 2.0 V +/- 0.1 V for Ti/SnO2-Sb2O5 electrode to oxidize organic compounds, while the optimum cathodic potential was -0.65 V for graphite electrode to reduce O2 generating H2O2. The oxidation degradation of aniline could not take place only by the single action of H2O2. Anodic oxidation was accounted for the degradation of aniline in the absence of Fe2+, while in the presence of Fe2+ both electro-Fenton oxidation and anodic oxidation (dual-electrode electrochemical oxidation) could degradate aniline effectively, and in this case the former was the main mechanism. Under the conditions of -0.65 V cathodic potential, pH 3.0 and 0.5 mmol x L(-1) Fe2+, the removal rate of COD was 77.5% after 10 h treatment and a current efficiency of 97.8% for COD removal could be obtained. This work indicates that the dual-electrode electrochemical oxidation is feasible for the degradation of organic compounds with a high current efficiency by using Ti/SnO2-Sb2O5 as anode as well as the reasonable anodic and cathodic potentials.

  20. Graphene electrode modified with electrochemically reduced graphene oxide for label-free DNA detection.

    PubMed

    Li, Bing; Pan, Genhua; Avent, Neil D; Lowry, Roy B; Madgett, Tracey E; Waines, Paul L

    2015-10-15

    A novel printed graphene electrode modified with electrochemically reduced graphene oxide was developed for the detection of a specific oligonucleotide sequence. The graphene oxide was immobilized onto the surface of a graphene electrode via π-π bonds and electrochemical reduction of graphene oxide was achieved by cyclic voltammetry. A much higher redox current was observed from the reduced graphene oxide-graphene double-layer electrode, a 42% and 36.7% increase, respectively, in comparison with that of a bare printed graphene or reduced graphene oxide electrode. The good electron transfer activity is attributed to a combination of the large number of electroactive sites in reduced graphene oxide and the high conductivity nature of graphene. The probe ssDNA was further immobilized onto the surface of the reduced graphene oxide-graphene double-layer electrode via π-π bonds and then hybridized with its target cDNA. The change of peak current due to the hybridized dsDNA could be used for quantitative sensing of DNA concentration. It has been demonstrated that a linear range from 10(-7)M to 10(-12)M is achievable for the detection of human immunodeficiency virus 1 gene with a detection limit of 1.58 × 10(-13)M as determined by three times standard deviation of zero DNA concentration. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Elementary reaction modeling of solid oxide electrolysis cells: Main zones for heterogeneous chemical/electrochemical reactions

    NASA Astrophysics Data System (ADS)

    Li, Wenying; Shi, Yixiang; Luo, Yu; Cai, Ningsheng

    2015-01-01

    A theoretical model of solid oxide electrolysis cells considering the heterogeneous elementary reactions, electrochemical reactions and the transport process of mass and charge is applied to study the relative performance of H2O electrolysis, CO2 electrolysis and CO2/H2O co-electrolysis and the competitive behavior of heterogeneous chemical and electrochemical reactions. In cathode, heterogeneous chemical reactions exist near the outside surface and the electrochemical reactions occur near the electrolyte. According to the mathematical analysis, the mass transfer flux D ∇c determines the main zone size of heterogeneous chemical reactions, while the charge transfer flux σ ∇V determines the other one. When the zone size of heterogeneous chemistry is enlarged, more CO2 could react through heterogeneous chemical pathway, and polarization curves of CO2/H2O co-electrolysis could be prone to H2O electrolysis. Meanwhile, when the zone size of electrochemistry is enlarged, more CO2 could react through electrochemical pathway, and polarization curves of CO2/H2O co-electrolysis could be prone to CO2 electrolysis. The relative polarization curves, the ratio of CO2 participating in electrolysis and heterogeneous chemical reactions, the mass and charge transfer flux and heterogeneous chemical/electrochemical reaction main zones are simulated to study the effects of cathode material characteristics (porosity, particle diameter and ionic conductivity) and operating conditions (gas composition and temperature).

  2. Occurrence and Removal of Organic Micropollutants in Landfill Leachates Treated by Electrochemical Advanced Oxidation Processes.

    PubMed

    Oturan, Nihal; van Hullebusch, Eric D; Zhang, Hui; Mazeas, Laurent; Budzinski, Hélène; Le Menach, Karyn; Oturan, Mehmet A

    2015-10-20

    In recent years, electrochemical advanced oxidation processes have been shown to be an effective alternative for the removal of refractory organic compounds from water. This study is focused on the effective removal of recalcitrant organic matter (micropollutants, humic substances, etc.) present in municipal solid waste landfill leachates. A mixture of eight landfill leachates has been studied by the electro-Fenton process using a Pt or boron-doped diamond (BDD) anode and a carbon felt cathode or by the anodic oxidation process with a BDD anode. These processes exhibit great oxidation ability due to the in situ production of hydroxyl radicals ((•)OH), a highly powerful oxidizing species. Both electrochemical processes were shown to be efficient in the removal of dissolved total organic carbon (TOC) from landfill leachates. Regarding the electro-Fenton process, the replacement of the classical anode Pt by the anode BDD allows better performance in terms of dissolved TOC removal. The occurrence and removal yield of 19 polycyclic aromatic hydrocarbons, 15 volatile organic compounds, 7 alkylphenols, 7 polychlorobiphenyls, 5 organochlorine pesticides, and 2 polybrominated diphenyl ethers in landfill leachate were also investigated. Both electrochemical processes allow one to reach a quasicomplete removal (about 98%) of these organic micropollutants.

  3. Destruction of commercial pesticides by cerium redox couple mediated electrochemical oxidation process in continuous feed mode.

    PubMed

    Balaji, Subramanian; Chung, Sang Joon; Ryu, Jae-Yong; Moon, Il Shik

    2009-12-30

    Mediated electrochemical oxidation was carried out for the destruction of commercial pesticide formulations using cerium(IV) in nitric acid as the mediator electrolyte solution in a bench scale set up. The mediator oxidant was regenerated in situ using an electrochemical cell. The real application of this sustainable process for toxic organic pollutant destruction lies in its ability for long term continuous operation with continuous organic feeding and oxidant regeneration with feed water removal. In this report we present the results of fully integrated MEO system. The task of operating the continuous feed MEO system for a long time was made possible by continuously removing the feed water using an evaporator set up. The rate of Ce(IV) regeneration in the electrochemical cell and the consumption for the pesticide destruction was matched based on carbon content of the pesticides. It was found that under the optimized experimental conditions for Ce(III) oxidation, organic addition and water removal destruction efficiency of ca. 99% was obtained for all pesticides studied. It was observed that the Ce(IV) concentration was maintained nearly the same throughout the experiment. The stable operation for 6h proved that the process can be used for real applications and for possible scale up for the destruction of larger volumes of toxic organic wastes.

  4. Treatment of papermaking tobacco sheet wastewater by electrocoagulation combined with electrochemical oxidation.

    PubMed

    Ma, Xiangjuan; Gao, Yang; Huang, Hanping

    2015-01-01

    Attempts were made in this study to examine the efficiency of electrocoagulation (EC) using aluminum (Al) anode and stainless steel net cathode combined with electrochemical oxidation with a β-PbO₂anode or a mixed metal oxide (MMO) anode for treatment of papermaking tobacco sheet wastewater, which has the characteristics of high content of suspended solids (SS), intensive color, and low biodegradability. The wastewater was first subjected to the EC process under 40 mA/cm² of current density, 2.5 g/L of NaCl, and maintaining the original pH of wastewater. After 6 minutes of EC process, the effluent was further treated by electrochemical oxidation. The results revealed that the removal of SS during the EC process was very beneficial to mass transfer of organics during electrochemical oxidation. After the combined process, 83.9% and 82.8% of chemical oxygen demand (COD) removal could be achieved on the β-PbO₂and MMO anodes, respectively. The main components of the final effluent were biodegradable organic acids, such as acetic acid, propionic acid, butyric acid, valeric acid, and hexahyl carbonic acid; the 5-day biochemical oxygen demand/chemical oxygen demand (BOD₅/COD) ratio increased from 0.06 to 0.85 (Al + β-PbO₂) or 0.80 (Al + MMO). Therefore, this integrated process is a promising alternative for pretreatment of papermaking tobacco sheet wastewater prior to biological treatment.

  5. Preparation and activation of micro-arc oxidation films on a TLM titanium alloy.

    PubMed

    Yu, S; Yu, Z T

    2008-12-01

    In order to improve the biocompatibility and surface activity of a TLM alloy, a layer of a porous TiO(2) film was prepared by the micro-arc oxidation method on the surface, and then the NH(-)(2) active group was introduced on the film by an activation treatment in an aminated solution. The phase identification and surface characteristics of the micro-arc oxidation films were characterized by XRD, XPS, SEM and EDS. The in vitro blood compatibility of the TLM alloy samples with and without surface modification was evaluated by contact angle tests, hemolysis tests and electrochemical tests. The results indicate that the biocompatibility and surface activity of the TLM alloy could be remarkably improved by surface modification of micro-arc oxidation and activation treatment.

  6. Preparation and activation of micro-arc oxidation films on a TLM titanium alloy

    NASA Astrophysics Data System (ADS)

    Yu, S.; Yu, Z. T.

    2008-12-01

    In order to improve the biocompatibility and surface activity of a TLM alloy, a layer of a porous TiO2 film was prepared by the micro-arc oxidation method on the surface, and then the NH-2 active group was introduced on the film by an activation treatment in an aminated solution. The phase identification and surface characteristics of the micro-arc oxidation films were characterized by XRD, XPS, SEM and EDS. The in vitro blood compatibility of the TLM alloy samples with and without surface modification was evaluated by contact angle tests, hemolysis tests and electrochemical tests. The results indicate that the biocompatibility and surface activity of the TLM alloy could be remarkably improved by surface modification of micro-arc oxidation and activation treatment.

  7. Effect of reaction temperature on carbon films prepared by a hydrothermal electrochemical method

    NASA Astrophysics Data System (ADS)

    Tao, Y.; Yi, D.; Zhu, B.

    2012-03-01

    Carbon films were synthesized under hydrothermal electrochemical conditions using sugar as the carbon source at temperature ranging from 170 °C to 180 °C. The reaction temperature affects the degree of sugar decomposition, the concentration of carbon ions, supersaturation and overpotential of the solution, thereby affecting the morphology, orientation, and crystallinity of the films. The graphitic content (sp2) increases with increasing the processing temperature and vice versa. The higher the synthesizing temperature the less the amount of amorphous carbon (sp3). The graphite in thin films prepared at 170 °C and 175 °C shows a (101) preferred orientation, whereas those prepared at 180 °C show a fairly random orientation. The mechanism of this synthesizing process seems to consist of three stages.

  8. Hollow CuO nanospheres uniformly anchored on porous Si nanowires: preparation and their potential use as electrochemical sensors.

    PubMed

    Guo, Zheng; Seol, Myeong-Lok; Kim, Moon-Seok; Ahn, Jae-Hyuk; Choi, Yang-Kyu; Liu, Jin-Huai; Huang, Xing-Jiu

    2012-12-07

    Hollow CuO nanospheres have been prepared via a reduction reaction of copper ions on porous Si nanowires combined with calcination in air and uniformly anchored on their surfaces. Scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) were employed to characterize and analyze as-synthesized samples. The results reveal that Si nanowires fabricated from heavily doped Si wafer are formed with a meso-porous structure by an Ag-assisted etching approach, and Cu nanoparticles are formed and uniformly decorated on the Si nanowires through a reaction of copper ions reduced by silicon. After annealing in air, Cu nanoparticles are in situ oxidized and transformed into CuO, leading to the formation of hollow nanospheres because of the Kirkendall effect. The diameter size of as-prepared CuO hollow spheres anchored on porous Si nanowires is mainly around 30 nm. Finally, in order to illuminate the advantages of this novel hybrid nanostructure of nanosized hollow spheres supported on porous nanowires, its electrochemical sensing performance to hydrazine as an example has been further investigated. The results confirm that it is a good potential application to detect hydrazine.

  9. Alzheimer's disease amyloid beta peptides in vitro electrochemical oxidation.

    PubMed

    Enache, Teodor Adrian; Oliveira-Brett, Ana Maria

    2017-04-01

    The oxidative behaviour of the human amyloid beta (Aβ1-40 and Aβ1-42) peptides and a group of similar peptides: control inverse (Aβ40-1 and Aβ42-1), mutants (Aβ1-40Phe(10) and Aβ1-40Nle(35)), rat Aβ1-40Rat, and fragments (Aβ1-28, Aβ1-16, Aβ10-20, Aβ12-28, and Aβ17-42), in solution or adsorbed, at a glassy carbon electrode, by cyclic and differential pulse voltammetry, were investigated and compared. Structurally the Aβ1-40 and Aβ1-42 sequences contain five electroactive amino acid residues, one tyrosine (Tyr(10)), three histidines (His(6), His(13) and His(14)) and one methionine (Met(35)). The Aβ peptide 3D structure influenced the exposure of the redox residues to the electrode surface and their oxidation peak currents. Depending on the amino acid sequence length and content, the Aβ peptides gave one or two oxidation peaks. The first electron transfer reaction corresponded to the tyrosine amino acid residue oxidation, and the second to both histidines and methionine amino acid residues. The highest contribution to the second oxidation peak current was from His(13), followed by His(14) and His(6) residues, and Met(35) residue had the lowest contribution. The Aβ peptides electron transfer depended on peptide hydrophobicity and 3D structure, the redox residues position in the sequence, the redox residues close to N-termini giving the highest oxidation peak currents.

  10. Direct Electrochemical Preparation of Cobalt, Tungsten, and Tungsten Carbide from Cemented Carbide Scrap

    NASA Astrophysics Data System (ADS)

    Xiao, Xiangjun; Xi, Xiaoli; Nie, Zuoren; Zhang, Liwen; Ma, Liwen

    2017-02-01

    A novel process of preparing cobalt, tungsten, and tungsten carbide powders from cemented carbide scrap by molten salt electrolysis has been investigated in this paper. In this experiment, WC-6Co and NaCl-KCl salt were used as sacrificial anode and electrolyte, respectively. The dissolution potential of cobalt and WC was determined by linear sweep voltammetry to be 0 and 0.6 V ( vs Ag/AgCl), respectively. Furthermore, the electrochemical behavior of cobalt and tungsten ions was investigated by a variety of electrochemical techniques. Results of cyclic voltammetry (CV) and square-wave voltammetry show that the cobalt and tungsten ions existed as Co2+ and W2+ on melts, respectively. The effect of applied voltage, electrolysis current, and electrolysis times on the composition of the product was studied. Results showed that pure cobalt powder can be obtained when the electrolysis potential is lower than 0.6 V or during low current and short times. Double-cathode and two-stage electrolysis was utilized for the preparation of cobalt, tungsten carbide, and tungsten powders. Additionally, X-ray diffraction results confirm that the product collected at cathodes 1 and 2 is pure Co and WC, respectively. Pure tungsten powder was obtained after electrolysis of the second part. Scanning electron microscope results show that the diameters of tungsten, tungsten carbide, and cobalt powder are smaller than 100, 200, and 200 nm, respectively.

  11. Chemical and electrochemical oxidation of small organic molecules

    NASA Astrophysics Data System (ADS)

    Smart, Marshall C.

    Direct oxidation fuel cells using proton-exchange membrane electrolytes have long been recognized as being an attractive mode of power generation. The current work addresses the electro-oxidation characteristics of a number of potential fuels on Pt-based electrodes which can be used in direct oxidation fuel cells, including hydrocarbons and oxygenated molecules, such as alcohols, formates, ethers, and acetals. Promising alternative fuels which were identified, such as trimethoxymethane and dimethoxymethane, were then investigated in liquid-feed PEM-based fuel cells. In addition to investigating the nature of the anodic electro-oxidation of organic fuels, effort was also devoted to developing novel polymer electrolyte membranes which have low permeability to organic molecules, such as methanol. This research was initiated with the expectation of reducing the extent of fuel crossover from the anode to the cathode in the liquid-feed design fuel cell which results in lower fuel efficiency and performance. Other work involving efforts to improve the performance of direct oxidation fuel cell includes research focused upon improving the kinetics of oxygen reduction. There is continued interest in the identification of new, safe, non-toxic, and inexpensive reagents which can be used in the oxidation of organic compounds. Urea-hydrogen peroxide (UHP), a hydrogen bonded adduct, has been shown to serve as a valuable source of hydrogen peroxide in a range of reactions. UHP has been shown to be ideal for the monohydroxylation of aromatics, including toluene, ethylbenzene, p-xylene, m-xylene, and mesitylene, as well as benzene, in the presence of trifluoromethanesulfonic acid. It was also found that aniline was converted to a mixture containing primarily azobenzene, azoxybenzene and nitrobenzene when reacted with UHP in glacial acetic acid. A number of aniline derivatives have been investigated and it was observed that the corresponding azoxybenzene derivatives could be

  12. Preparing oxidizer coated metal fuel particles

    NASA Technical Reports Server (NTRS)

    Shafer, J. I.; Simmons, G. M. (Inventor)

    1974-01-01

    A solid propellant composition of improved efficiency is described which includes an oxidizer containing ammonium perchlorate, and a powered metal fuel, preferably aluminum or beryllium, in the form of a composite. The metal fuel is contained in the crystalline lattice framework of the oxidizer, as well as within the oxidizer particles, and is disposed in the interstices between the oxidizer particles of the composition. The propellant composition is produced by a process comprising the crystallization of ammonium perchlorate in water, in the presence of finely divided aluminum or beryllium. A suitable binder is incorporated in the propellant composition to bind the individual particles of metal with the particles of oxidizer containing occluded metal.

  13. Indium Tin Oxide Nanoparticles/Vaseline Nanocomposites: Preparation of Nanoelectrode Assembles with Tunable Dimensions.

    PubMed

    Lin, Yuqing; Yin, Lu; Xu, Yanan; Gao, Yuelei

    2015-03-01

    In this paper, we describe a novel approach for fabricating tailor-made indium tin oxide nanoelectrode assembles (ITO-NEAs) based on indium tin oxide nanoparticles (ITONPs) as conducting materials and vaseline as insulating binder. ITO nanoelectrode assembles were formed on the surface of a glassy carbon electrode (GCE) by uniformly covering GCE with ITONPs/vaseline nanocomposite. Cyclic voltammetry (CV) studies demonstrated that the ITO-NEAs exhibit fast mass transport and low charging current, suggesting that the ITO-NEAs, fabricated with ITONPs and vaseline hybrid film coating, behave like a microelectrode array. Furthermore, electrochemical results show the as-prepared ITONPs electrodes have tunable dimensions, ranging from a conventional electrode to a nanoelectrode ensemble, depending on the amount of insulting vaseline dissolved in the ITO-NPs/acetone dispersion. As novel kind of ITONPs-based film electrodes with tunable dimensions and good electrochemical activity, the ITO film electrodes are very attractive for potential application in fundamental and practical electrochemical studies.

  14. Zn2+-Doped Polyaniline/Graphene Oxide as Electrode Material for Electrochemical Supercapacitors

    NASA Astrophysics Data System (ADS)

    Xu, Hui; Tang, Jing; Chen, Yong; Liu, Jian; Pu, Jinjuan; Li, Qi

    2017-10-01

    Electrodes based on Zn2+-doped polyaniline/graphene oxide (Zn2+/PANI/GO) were synthesized on stainless steel mesh substrates in H2SO4 solution via electrochemical codeposition. Different concentrations of graphene oxide (GO) were incorporated into the films to improve the electrochemical performance of the electrodes. Electrochemical properties of the films were tested by cyclic voltammetry, galvanostatic charge-discharge tests, and electrochemical impedance spectroscopy, in a three-electrode system. The maximum specific capacitance of the Zn2+/PANI/GO film with a GO concentration of 15 mg L-1 was found to be 1266 F g-1 at a scan rate of 3 mV s-1. This value was higher than that of a Zn2+ doped polyaniline (Zn2+/PANI) film (814 F g-1). The Zn2+/PANI/GO film also showed good cycling stability, retaining over 86% of its initial capacitance after 1000 cycles. These results indicate that the Zn2+/PANI/GO composites can be applied as high performance supercapacitor electrodes.

  15. Electrochemical Alcohol Oxidation Mediated by TEMPO‐like Nitroxyl Radicals

    PubMed Central

    Ciriminna, Rosaria; Ghahremani, Mina

    2017-01-01

    Abstract The electrocatalytic oxidation of alcohols mediated by TEMPO‐like nitroxyl radicals is an economically and industrially viable method that will shortly find commercial application in the synthesis of valued substances including active pharmaceutical ingredients (APIs), valued natural product derivatives, fine chemicals, and valued nanomaterials. PMID:28168142

  16. Electrochemically deposited gallium oxide nanostructures on silicon substrates.

    PubMed

    Ghazali, Norizzawati Mohd; Mahmood, Mohamad Rusop; Yasui, Kanji; Hashim, Abdul Manaf

    2014-03-17

    We report a synthesis of β-Ga2O3 nanostructures on Si substrate by electrochemical deposition using a mixture of Ga2O3, HCl, NH4OH, and H2O. The presence of Ga3+ ions contributed to the deposition of Ga2O3 nanostructures on the Si surface with the assistance of applied potentials. The morphologies of the grown structures strongly depended on the molarity of Ga2O3 and pH level of electrolyte. β-Ga2O3 nanodot-like structures were grown on Si substrate at a condition with low molarity of Ga2O3. However, Ga2O3 nanodot structures covered with nanorods on top of their surfaces were obtained at higher molarity, and the densities of nanorods seem to increase with the decrease of pH level. High concentration of Ga3+ and OH- ions may promote the reaction of each other to produce Ga2O3 nanorods in the electrolyte. Such similar nature of Ga2O3 nanorods was also obtained by using hydrothermal process. The grown structures seem to be interesting for application in electronic and optoelectronic devices as well as to be used as a seed structure for subsequent chemical synthesis of GaN by thermal transformation method.

  17. Electrochemically deposited gallium oxide nanostructures on silicon substrates

    NASA Astrophysics Data System (ADS)

    Ghazali, Norizzawati Mohd; Mahmood, Mohamad Rusop; Yasui, Kanji; Hashim, Abdul Manaf

    2014-03-01

    We report a synthesis of β-Ga2O3 nanostructures on Si substrate by electrochemical deposition using a mixture of Ga2O3, HCl, NH4OH, and H2O. The presence of Ga3+ ions contributed to the deposition of Ga2O3 nanostructures on the Si surface with the assistance of applied potentials. The morphologies of the grown structures strongly depended on the molarity of Ga2O3 and pH level of electrolyte. β-Ga2O3 nanodot-like structures were grown on Si substrate at a condition with low molarity of Ga2O3. However, Ga2O3 nanodot structures covered with nanorods on top of their surfaces were obtained at higher molarity, and the densities of nanorods seem to increase with the decrease of pH level. High concentration of Ga3+ and OH- ions may promote the reaction of each other to produce Ga2O3 nanorods in the electrolyte. Such similar nature of Ga2O3 nanorods was also obtained by using hydrothermal process. The grown structures seem to be interesting for application in electronic and optoelectronic devices as well as to be used as a seed structure for subsequent chemical synthesis of GaN by thermal transformation method.

  18. Electrochemically deposited gallium oxide nanostructures on silicon substrates

    PubMed Central

    2014-01-01

    We report a synthesis of β-Ga2O3 nanostructures on Si substrate by electrochemical deposition using a mixture of Ga2O3, HCl, NH4OH, and H2O. The presence of Ga3+ ions contributed to the deposition of Ga2O3 nanostructures on the Si surface with the assistance of applied potentials. The morphologies of the grown structures strongly depended on the molarity of Ga2O3 and pH level of electrolyte. β-Ga2O3 nanodot-like structures were grown on Si substrate at a condition with low molarity of Ga2O3. However, Ga2O3 nanodot structures covered with nanorods on top of their surfaces were obtained at higher molarity, and the densities of nanorods seem to increase with the decrease of pH level. High concentration of Ga3+ and OH- ions may promote the reaction of each other to produce Ga2O3 nanorods in the electrolyte. Such similar nature of Ga2O3 nanorods was also obtained by using hydrothermal process. The grown structures seem to be interesting for application in electronic and optoelectronic devices as well as to be used as a seed structure for subsequent chemical synthesis of GaN by thermal transformation method. PMID:24629107

  19. Amorphous thin film ruthenium oxide as an electrode material for electrochemical capacitors

    SciTech Connect

    Jow, T.R.; Zheng, J.P.

    1995-12-31

    Ruthenium oxide thin films of an amorphous phase were successfully prepared on a titanium (Ti) substrate at temperatures below 160 C. The sol-gel process using metal alkoxide precursor in nonaqueous solvents was used to prepare these films. The preliminary results showed that a specific capacitance of 430 F/g can be achieved for amorphous ruthenium oxide electrode in sulfuric acid. Films prepared by this method are compared with the films prepared by the thermal decomposition of the aqueous ruthenium chloride solution at temperatures above 300 C. The specific capacitance, the crystalline structure, and the surface morphology of these films as a function of the preparation temperature were also discussed.

  20. A highly sensitive electrochemical biosensor for catechol using conducting polymer reduced graphene oxide-metal oxide enzyme modified electrode.

    PubMed

    Sethuraman, V; Muthuraja, P; Anandha Raj, J; Manisankar, P

    2016-10-15

    The fabrication, characterization and analytical performances were investigated for a catechol biosensor, based on the PEDOT-rGO-Fe2O3-PPO composite modified glassy carbon (GC) electrode. The graphene oxide (GO) doped conducting polymer poly (3,4-ethylenedioxythiophene) (PEDOT) was prepared through electrochemical polymerization by potential cycling. Reduction of PEDOT-GO was carried out by amperometric method. Fe2O3 nanoparticles were synthesized in ethanol by hydrothermal method. The mixture of Fe2O3, PPO and glutaraldehyde was casted on the PEDOT-rGO electrode. The surface morphology of the modified electrodes was studied by FE-SEM and AFM. Cyclic voltammetric studies of catechol on the enzyme modified electrode revealed higher reduction peak current. Determination of catechol was carried out successfully by Differential Pulse Voltammetry (DPV) technique. The fabricated biosensor investigated shows a maximum current response at pH 6.5. The catechol biosensor exhibited wide sensing linear range from 4×10(-8) to 6.20×10(-5)M, lower detection limit of 7×10(-9)M, current maxima (Imax) of 92.55µA and Michaelis-Menten (Km) constant of 30.48µM. The activation energy (Ea) of enzyme electrode is 35.93KJmol(-1) at 50°C. There is no interference from d-glucose and l-glutamic acid, ascorbic acid and o-nitrophenol. The PEDOT-rGO-Fe2O3-PPO biosensor was stable for at least 75 days when stored in a buffer at about 4°C.

  1. Facile synthesis of cuprous oxide nanowires decorated graphene oxide nanosheets nanocomposites and its application in label-free electrochemical immunosensor.

    PubMed

    Wang, Huan; Zhang, Yong; Wang, Yulan; Ma, Hongmin; Du, Bin; Wei, Qin

    2017-01-15

    In this work, the assembly between one-dimensional (1D) nanomaterials and two-dimensional (2D) nanomaterials was achieved by a simple method. Cuprous oxide nanowires decorated graphene oxide nanosheets (Cu2O@GO) nanocomposites were synthesized for the first time by a simple electrostatic self-assembly process. The nanostructure was well confirmed by scanning electron microscope (SEM) and transmission electron microscope (TEM) images. Taking advantages of good electrocatalytic activity and high specific surface area of Cu2O@GO nanocomposites, a label-free electrochemical immunosensor was developed by employing Cu2O@GO as signal amplification platform for the quantitative detection of alpha fetoprotein (AFP). In addition, toluidine blue (TB) was used as the electron transfer mediator to provide the electrochemical signal, which was adsorbed on graphene oxide nanosheets (GO NSs) by electrostatic attraction. The detection mechanism was based on the monitoring of the electrochemical current response change of TB by the square wave voltammetry (SWV) when immunoreaction occurred on the surface of electrode. Under optimal conditions, the proposed immunosensor displayed a high sensitivity and a low detection limit. This designed method may provide an effective method in the clinical diagnosis of AFP and other tumor markers.

  2. Post-treatment of reclaimed waste water based on an electrochemical advanced oxidation process

    NASA Technical Reports Server (NTRS)

    Verostko, Charles E.; Murphy, Oliver J.; Hitchens, G. D.; Salinas, Carlos E.; Rogers, Tom D.

    1992-01-01

    The purification of reclaimed water is essential to water reclamation technology life-support systems in lunar/Mars habitats. An electrochemical UV reactor is being developed which generates oxidants, operates at low temperatures, and requires no chemical expendables. The reactor is the basis for an advanced oxidation process in which electrochemically generated ozone and hydrogen peroxide are used in combination with ultraviolet light irradiation to produce hydroxyl radicals. Results from this process are presented which demonstrate concept feasibility for removal of organic impurities and disinfection of water for potable and hygiene reuse. Power, size requirements, Faradaic efficiency, and process reaction kinetics are discussed. At the completion of this development effort the reactor system will be installed in JSC's regenerative water recovery test facility for evaluation to compare this technique with other candidate processes.

  3. Post-treatment of reclaimed waste water based on an electrochemical advanced oxidation process

    NASA Technical Reports Server (NTRS)

    Verostko, Charles E.; Murphy, Oliver J.; Hitchens, G. D.; Salinas, Carlos E.; Rogers, Tom D.

    1992-01-01

    The purification of reclaimed water is essential to water reclamation technology life-support systems in lunar/Mars habitats. An electrochemical UV reactor is being developed which generates oxidants, operates at low temperatures, and requires no chemical expendables. The reactor is the basis for an advanced oxidation process in which electrochemically generated ozone and hydrogen peroxide are used in combination with ultraviolet light irradiation to produce hydroxyl radicals. Results from this process are presented which demonstrate concept feasibility for removal of organic impurities and disinfection of water for potable and hygiene reuse. Power, size requirements, Faradaic efficiency, and process reaction kinetics are discussed. At the completion of this development effort the reactor system will be installed in JSC's regenerative water recovery test facility for evaluation to compare this technique with other candidate processes.

  4. Strongly improved electrochemical cycling durability by adding iridium to electrochromic nickel oxide films.

    PubMed

    Wen, Rui-Tao; Niklasson, Gunnar A; Granqvist, Claes G

    2015-05-13

    Anodically colored nickel oxide (NiO) thin films are of much interest as counter electrodes in tungsten oxide based electrochromic devices such as "smart windows" for energy-efficient buildings. However, NiO films are prone to suffering severe charge density degradation upon prolonged electrochemical cycling, which can lead to insufficient device lifetime. Therefore, a means to improve the durability of NiO-based films is an important challenge at present. Here we report that the incorporation of a modest amount of iridium into NiO films [Ir/(Ir + Ni) = 7.6 atom %] leads to remarkable durability, exceeding 10000 cycles in a lithium-conducting electrolyte, along with significantly improved optical modulation during extended cycling. Structure characterization showed that the face-centered-cubic-type NiO structure remained after iridium addition. Moreover, the crystallinity of these films was enhanced upon electrochemical cycling.

  5. A Molecularly Imprinted Polymer with Incorporated Graphene Oxide for Electrochemical Determination of Quercetin

    PubMed Central

    Sun, Si; Zhang, Mengqi; Li, Yijun; He, Xiwen

    2013-01-01

    The molecularly imprinted polymer based on polypyrrole film with incorporated graphene oxide was fabricated and used for electrochemical determination of quercetin. The electrochemical behavior of quercetin on the modified electrode was studied in detail using differential pulse voltammetry. The oxidation peak current of quercetin in B-R buffer solution (pH = 3.5) at the modified electrode was regressed with the concentration in the range from 6.0 × 10−7 to 1.5 × 10−5 mol/L (r2 = 0.997) with a detection limit of 4.8 × 10−8 mol/L (S/N = 3). This electrode showed good stability and reproducibility. In the above mentioned range, rutin or morin which has similar structures and at the same concentration as quercetin did not interfere with the determination of quercetin. The applicability of the method for complex matrix analysis was also evaluated. PMID:23698263

  6. Electrochemical properties of poly(vinyl alcohol) and graphene oxide composite for supercapacitor applications

    NASA Astrophysics Data System (ADS)

    Theophile, Niyitanga; Jeong, Hae Kyung

    2017-02-01

    Poly(vinyl alcohol), PVA, polymer was successfully combined with graphene oxide (GO) and thermally reduced graphene oxide (RGO), respectively, to make composites and characterized for supercapacitor applications. PVA-RGO composite shows excellent electrochemical properties compared to PVA-GO composite. The capacitance of 190 Fg-1 is obtained from PVA-RGO composite which is larger than that (13 Fg-1) of PVA-GO composite. Electrochemical impedance of PVA-RGO is more than ten times smaller than that of PVA-GO at 20 kHz, demonstrating that PVA-RGO composite has a great advantage for supercapacitor applications compared to PVA, GO, RGO, and PVA-GO composite.

  7. Imaging of a thin oxide film formation from the combination of surface reflectivity and electrochemical methods.

    PubMed

    Chakri, Sara; Patel, Anisha N; Frateur, Isabelle; Kanoufi, Frédéric; Sutter, Eliane Marie Madeleine; Tran, T T Mai; Tribollet, Bernard; Vivier, Vincent

    2017-04-13

    Electrochemical methods (cyclic voltammetry (CV), potential steps, and electrochemical impedance spectroscopy), were successfully combined with in situ reflectometry measurements for a detailed analysis of the passive layer evolution as a function of the electrode potential. Interestingly, both EIS and surface reflectivity allowed a film thickness in the nanometer range to be readily determined. In addition, transient analyses of the reflectivity simultaneously recorded with CVs show the formation of both Fe2O3 and Fe3O4 oxides. The image analysis showed that the steel surface reactivity is heterogeneous and presents micrometric islands coated with thicker oxide layer than the surrounding surface. The in situ combination of these techniques thus offers a powerful analytical description of the interface on local scale and its transient response to a perturbation.

  8. A molecularly imprinted polymer with incorporated graphene oxide for electrochemical determination of quercetin.

    PubMed

    Sun, Si; Zhang, Mengqi; Li, Yijun; He, Xiwen

    2013-04-25

    The molecularly imprinted polymer based on polypyrrole film with incorporated graphene oxide was fabricated and used for electrochemical determination of quercetin. The electrochemical behavior of quercetin on the modified electrode was studied in detail using differential pulse voltammetry. The oxidation peak current of quercetin in B-R buffer solution (pH = 3.5) at the modified electrode was regressed with the concentration in the range from 6.0 × 10(-7) to 1.5 × 10(-5) mol/L (r2 = 0.997) with a detection limit of 4.8 × 10(-8) mol/L (S/N = 3). This electrode showed good stability and reproducibility. In the above mentioned range, rutin or morin which has similar structures and at the same concentration as quercetin did not interfere with the determination of quercetin. The applicability of the method for complex matrix analysis was also evaluated.

  9. Electrochemical sensing of glucose by reduced graphene oxide-zinc ferrospinels

    NASA Astrophysics Data System (ADS)

    Shahnavaz, Zohreh; Woi, Pei Meng; Alias, Yatimah

    2016-08-01

    We have developed ZnFe2O4 magnetic nanoparticles/reduced graphene oxide nanosheets modified glassy carbon (ZnFe2O4/rGO/GCE) electrode as a novel system for the electrochemical glucose sensing. Via a facile in situ hydrothermal route, the reduction of GO and the formation of ZnFe2O4 nanoparticles occurred simultaneously. This enables the ZnFe2O4 nanoparticles dispersed on the reduced graphene sheet. Characterization of nanocomposite by X-ray diffraction (XRD) and transmission electron microscopy (TEM) clearly demonstrate the successful attachment of ZnFe2O4 nanoparticles to graphene sheets. Electrochemical studies revealed that the ZnFe2O4/rGO/GCE possess excellent electrocatalytic activities toward the oxidation of glucose and the performance of sensor is enhanced by integration of graphene nanosheets with ZnFe2O4 nanoparticles.

  10. An electrochemical approach to graphene oxide coated sulfur for long cycle life

    NASA Astrophysics Data System (ADS)

    Moon, Joonhee; Park, Jungjin; Jeon, Cheolho; Lee, Jouhahn; Jo, Insu; Yu, Seung-Ho; Cho, Sung-Pyo; Sung, Yung-Eun; Hong, Byung Hee

    2015-07-01

    Owing to the possibilities of achieving high theoretical energy density and gravimetric capacity, sulfur has been considered as a promising cathode material for rechargeable lithium batteries. However, sulfur shows rapid capacity fading due to the irreversible loss of soluble polysulfides and the decrease in active sites needed for conducting agents. Furthermore, the low electrical conductivity of sulfur hampers the full utilization of active materials. Here we report that graphene oxide coated sulfur composites (GO-S/CB) exhibit improved electrochemical stability as well as enhanced rate performance, evidenced by various electrochemical analyses. The cyclic voltammetry and the galvanostatic cycling analysis revealed that the GO plays key roles in homogenizing the nanocomposite structures of the electrodes, in improving the electrochemical contact, and in minimizing the loss of soluble polysulfide intermediates. An electrochemical impedance spectroscopy analysis also confirms the enhanced structural stability of the GO-S/CB composites after battery operation. As a result, the GO-S/CB exhibited excellent cycle stability and specific capacity as high as ~723.7 mA h g-1 even after 100 cycles at 0.5 C.Owing to the possibilities of achieving high theoretical energy density and gravimetric capacity, sulfur has been considered as a promising cathode material for rechargeable lithium batteries. However, sulfur shows rapid capacity fading due to the irreversible loss of soluble polysulfides and the decrease in active sites needed for conducting agents. Furthermore, the low electrical conductivity of sulfur hampers the full utilization of active materials. Here we report that graphene oxide coated sulfur composites (GO-S/CB) exhibit improved electrochemical stability as well as enhanced rate performance, evidenced by various electrochemical analyses. The cyclic voltammetry and the galvanostatic cycling analysis revealed that the GO plays key roles in homogenizing the

  11. Electrochemical reaction and oxidation of lecithin under pulsed electric fields (PEF) processing.

    PubMed

    Zhao, Wei; Yang, Ruijin; Liang, Qi; Zhang, Wenbin; Hua, Xiao; Tang, Yali

    2012-12-12

    Pulsed electric fields (PEF) processing is a promising nonthermal food preservation technology, which is ongoing from laboratory and pilot plant scale levels to the industrial level. Currently, greater attention has been paid to side effects occurring during PEF treatment and the influences on food qualities and food components. The present study investigated the electrochemical reaction and oxidation of lecithin under PEF processing. Results showed that electrochemical reaction of NaCl solutions at different pH values occurred during PEF processing. Active chlorine, reactive oxygen, and free radicals were detected, which were related to the PEF parameters and pH values of the solution. Lecithin extracted from yolk was further selected to investigate the oxidation of food lipids under PEF processing, confirming the occurrence of oxidation of lecithin under PEF treatment. The oxidative agents induced by PEF might be responsible for the oxidation of extracted yolk lecithin. Moreover, this study found that vitamin C as a natural antioxidant could effectively quench free radicals and inhibit the oxidation of lipid in NaCl and lecithin solutions as model systems under PEF processing, representing a way to minimize the impact of PEF treatment on food qualities.

  12. Electrochemical oxidation of COD from real textile wastewaters: Kinetic study and energy consumption.

    PubMed

    Zou, Jiaxiu; Peng, Xiaolan; Li, Miao; Xiong, Ying; Wang, Bing; Dong, Faqin; Wang, Bin

    2017-03-01

    In the present study, the electrochemical oxidation of real wastewaters discharged by textile industry was carried out using a boron-doped diamond (BDD) anode. The effect of operational variables, such as applied current density (20-100 mA·cm(-2)), NaCl concentration added to the real wastewaters (0-3 g·L(-1)), and pH value (2.0-10.0), on the kinetics of COD oxidation and on the energy consumption was carefully investigated. The obtained experimental results could be well matched with a proposed kinetic model, in which the indirect oxidation mediated by electrogenerated strong oxidants would be described through a pseudo-first-order kinetic constant k. Values of k exhibited a linear increase with increasing applied current density and decreasing pH value, and an exponential increase with NaCl concentration. Furthermore, high oxidation kinetics resulted in low specific energy consumption, but this conclusion was not suitable to the results obtained under different applied current density. Under the optimum operational conditions, it only took 3 h to complete remove the COD in the real textile wastewaters and the specific energy consumption could be as low as 11.12 kWh·kg(-1) COD. The obtained results, low energy consumption and short electrolysis time, allowed to conclude that the electrochemical oxidation based on BDD anodes would have practical industrial application for the treatment of real textile wastewater.

  13. Electrochemical oxidation of cyanide in the hydrocyclone cell

    SciTech Connect

    Dhamo, N.

    1996-12-31

    A diluted electroplating cyanide rinse water has been used to test the use of the hydrocyclone cell (HCC) in batch recycle mode of operation for the simultaneous oxidation of cyanide during the electrodeposition of silver. The results obtained in this work with regard to the final products, current efficiency and the number of transferred electrons per CN{sup {minus}} helped to establish a probable reaction scheme. According to this, the process occurs mainly with one-electron transfer, through cyanate and cyanogen as intermediate species. Meanwhile, under conditions where the electrolyte circulates in an open bath and flows successively through the cathodic and the anodic compartments, as in the case of the HCC system, the cyanate could be produced by the direct oxidation through air and/or generated peroxide and CN could be lost as HCN (g).

  14. Simultaneous electrochemical determination of dopamine and paracetamol on multiwalled carbon nanotubes/graphene oxide nanocomposite-modified glassy carbon electrode.

    PubMed

    Cheemalapati, Srikanth; Palanisamy, Selvakumar; Mani, Veerappan; Chen, Shen-Ming

    2013-12-15

    In the present study, multiwalled carbon nanotubes (MWCNT)/graphene oxide (GO) nanocomposite was prepared by homogenous dispersion of MWCNT and GO and used for the simultaneous voltammetric determination of dopamine (DA) and paracetamol (PA). The TEM results confirmed that MWCNT walls were wrapped well with GO sheets. The MWCNT/GO nanocomposite showed superior electrocatalytic activity towards the oxidation of DA and PA, when compared with either pristine MWCNT or GO. The major reason for the efficient simultaneous detection of DA and PA at nanocomposite was the synergistic effect between MWCNT and GO. The electrochemical oxidation of DA and PA was investigated by cyclic voltammetry, differential pulse voltammetry and amperometry. The nanocomposite modified electrode showed electrocatalytic oxidation of DA and PA in the linear response range from 0.2 to 400 µmol L(-1) and 0.5 to 400 µmol L(-1) with the detection limit of 22 nmol L(-1) and 47 nmol L(-1) respectively. The proposed sensor displayed good selectivity, sensitivity, stability with appreciable consistency and precision.

  15. The electrochemical oxidation of chalcopyrite in ammoniacal solutions

    NASA Astrophysics Data System (ADS)

    Warren, G. W.; Wadsworth, M. E.

    1984-06-01

    The anodic dissolution of chalcopyrite in ammoniacal solutions was investigated using electrochemical methods. At low overvoltages, the formation of a copper deficient sulfide layer, Cu1-xFeS2 through a charge transfer reaction is proposed based upon the dependence of the rest or open circuit potential on solution composition and the presence of a Tafel region of appropriate slope. In addition, a current peak that occurs at 10-4 A/cm2 is a function of the square root of the voltage scanning speed and is explained in terms of a charge transfer reaction. At larger overvoltages, constant potential experiments and mass balances performed at various anodic potentials indicate that the dissolution is consistent with the overall reaction, CuFeS2 + 4NH3 + 9OH- = Cu(NH3){4/+2} + Fe(OH)3 + S2O{3/=} + 3H2O + 9e -, although some copper may be released to solution in the cuprous state and some ferrous iron has been identified in the product film. Current vs time data taken during constant potential experiments were found to obey a linear rate relationship. This was interpreted in terms of the formation of a layer of constant thickness which is corroded at the outer interface at the same rate it is formed at the inner interface.. The model proposed is typical of the corrosion of some metals. An examination of the polarization curves shows the dissolution reaction to be first order with respect to [OH-]. The lack of dependence on [Cu2+] indicates that the catalytic effect of cupric ion during oxygen pressure leaching is related only to the cathodic reduction of O2 in agreement with the results of previous investigations.

  16. Mediated electrochemical oxidation of organic wastes using a Co(III) mediator in a neutral electrolyte

    DOEpatents

    Balazs, G.B.; Lewis, P.R.

    1999-07-06

    An electrochemical cell with a Co(III) mediator and neutral pH anolyte provides efficient destruction of organic and mixed wastes. The organic waste is concentrated in the anolyte reservoir, where the cobalt mediator oxidizes the organics and insoluble radioactive species and is regenerated at the anode until all organics are converted to carbon dioxide and destroyed. The neutral electrolyte is non-corrosive, and thus extends the lifetime of the cell and its components. 2 figs.

  17. Mediated electrochemical oxidation of organic wastes using a Co(III) mediator in a neutral electrolyte

    DOEpatents

    Balazs, G. Bryan; Lewis, Patricia R.

    1999-01-01

    An electrochemical cell with a Co(III) mediator and neutral pH anolyte provides efficient destruction of organic and mixed wastes. The organic waste is concentrated in the anolyte reservoir, where the cobalt mediator oxidizes the organics and insoluble radioactive species and is regenerated at the anode until all organics are converted to carbon dioxide and destroyed. The neutral electrolyte is non-corrosive, and thus extends the lifetime of the cell and its components.

  18. Electrochemically oxidized electronic and ionic conducting nanostructured block copolymers for lithium battery electrodes.

    PubMed

    Patel, Shrayesh N; Javier, Anna E; Balsara, Nitash P

    2013-07-23

    Block copolymers that can simultaneously conduct electronic and ionic charges on the nanometer length scale can serve as innovative conductive binder material for solid-state battery electrodes. The purpose of this work is to study the electronic charge transport of poly(3-hexylthiophene)-b-poly(ethylene oxide) (P3HT-PEO) copolymers electrochemically oxidized with lithium bis(trifluoromethanesulfonyl) imide (LiTFSI) salt in the context of a lithium battery charge/discharge cycle. We use a solid-state three-terminal electrochemical cell that enables simultaneous conductivity measurements and control over electrochemical doping of P3HT. At low oxidation levels (ratio of moles of electrons removed to moles of 3-hexylthiophene moieties in the electrode), the electronic conductivity (σe,ox) increases from 10(-7) S/cm to 10(-4) S/cm. At high oxidation levels, σe,ox approaches 10(-2) S/cm. When P3HT-PEO is used as a conductive binder in a positive electrode with LiFePO4 active material, P3HT is electrochemically active within the voltage window of a charge/discharge cycle. The electronic conductivity of the P3HT-PEO binder is in the 10(-4) to 10(-2) S/cm range over most of the potential window of the charge/discharge cycle. This allows for efficient electronic conduction, and observed charge/discharge capacities approach the theoretical limit of LiFePO4. However, at the end of the discharge cycle, the electronic conductivity decreases sharply to 10(-7) S/cm, which means the "conductive" binder is now electronically insulating. The ability of our conductive binder to switch between electronically conducting and insulating states in the positive electrode provides an unprecedented route for automatic overdischarge protection in rechargeable batteries.

  19. Electrochemical oxidation of xanthosine. Isolation and structure elucidation of a new dimeric xanthine nucleoside

    SciTech Connect

    Xinhua Ji; Subramanian, P.; van der Helm, D.; Dryhurst, G. )

    1990-02-16

    Electrochemical oxidation of xanthosine (2) at pH 2 at a pyrolytic graphite electrode generates an electrophilic radical cation intermediate. Nucleophilic attack by 2 on this radical results, ultimately, in formation of 3-(8-xanthosyl)xanthosine (7). Hydrolytic cleavage of one ribose residue from 7 in acidic solution leads to 3-(8-xanthosyl)xanthine (8). The structure of 8, a new dimeric xanthine nucleoside, has been established using spectral and X-ray diffraction methods.

  20. Membrane electro-oxidizer: A new hybrid membrane system with electrochemical oxidation for enhanced organics and fouling control.

    PubMed

    Mameda, Naresh; Park, Hyung-June; Choo, Kwang-Ho

    2017-09-05

    The synergistic combination of membrane filtration with advanced oxidation is of particular interest for next-generation wastewater treatment technologies. A membrane electro-oxidizer (MEO) hybridizing a submerged microfilter and an electrochemical cell was developed and investigated for tertiary treatment of secondary industrial (textile) wastewater effluent. Laboratory- and pilot-scale MEO systems were designed and evaluated for treatment efficiency and membrane fouling control. The MEO achieved substantial removal of color (50-90%), turbidity (>90%), and bacteria (>4 log) as well as chemical oxygen demand (13-31%) and 1,4-dioxane (∼25-53%). Fluorescence-based parallel factor analysis disclosed the degradation of humic-like organics with fluorophores. Size exclusion chromatograms with organic carbon detection confirmed the removal of specific organic molecules with ∼100 Da. While investigating the effects of oxidant quenching agents, reactive chlorine species and hydrogen peroxide were found to be most responsible for the anodic oxidation of secondary effluent organics. The efficacy of membrane fouling mitigation by the MEO was greater when higher electric current densities were applied, but was not dependent on the number of electrochemical cells installed. The MEO is a promising technology for enhanced organics removal with simultaneous fouling control due to its multifunctional active oxidants. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Batch fabrication of mesoporous boron-doped nickel oxide nanoflowers for electrochemical capacitors

    SciTech Connect

    Yang, Jing-He; Yu, Qingtao; Li, Yamin; Mao, Liqun; Ma, Ding

    2014-11-15

    Highlights: • A new facile liquid-phase method has been employed for synthesis boron-doped NiO nanoflowers. • The specific surface area of NiO is as high as 200 m{sup 2} g{sup −1}. • NiO nanoflowers exhibit a high specific capacitance of ∼1309 F g{sup −1} at a charge and discharge current density of 3 A g{sup −1}. • NiO nanoflowers have excellent cycling ability and even after 2500 cycles there is no significant reduction in specific capacitance. - Abstract: Boron-doped nickel oxide (B-NiO) nanoflowers are prepared by simple thermal decomposition of nickel hydroxide. B-NiO is porous sphere with a diameter of about 400 nm. B-NiO nanoflowers are composed of approximately 30 nm nanoplates and the thickness of the nanosheets is approximately 3 nm. The specific surface area of the material is as high as 200 m{sup 2} g{sup −1} and the pore size distribution curves of B-NiO has three typical peaks in the range of mesoporous (5 nm, 13 nm and 18 nm). As an electrode for supercapacitors, the crystalline B-NiO nanoflowers have favorable characteristics, for instance, a specific capacitance of 1309 F g{sup −1} at a current density of 3 A g{sup −1} and no significant reduction in Coulombic efficiency after 2500 cycles at 37.5 A g{sup −1}. This remarkable electrochemical performance will make B-NiO nanoflowers a promising electrode material for high performance supercapacitors.

  2. COD and color removal of reactive orange 16 dye solution by electrochemical oxidation and adsorption method

    NASA Astrophysics Data System (ADS)

    Zakaria, Zuhailie; Ahmad, Wan Yaacob Wan; Yusop, Muhammad Rahimi; Othman, Mohamed Rozali

    2015-09-01

    Degradation of Reactive Orange 16 (RO16) dye was investigated using electrochemical oxidation and adsorption (batch method) using mixture of coconut trunk charcoal-graphite-tin-polyvinyl chloride(PVC). In batch studies for adsorbents pellet and powder form of the charcoal mixture were used. RO16 was chosen as the model dye because of its high resistance towards conventional treatment methods. NaCl and RO16 concentration, treatment duration, weight of electrode and adsorbent and volume of solution were kept constant for both methods. The effectiveness of the treatments were compared and evaluated by percentage of RO16 decolorization and chemical oxygen demand (COD) removal and results indicated that electrochemical oxidation method ables to decolorized RO16 dye up to 98.5% after 20 minutes electrolysis time while pellet and powder in batch method only removed 17.1 and 33.6% of RO16 color respectively. However, only 45.6% of COD can be removed using electrochemical oxidation method while pellet and powder in batch method removed 47.8 and 49.6% of COD respectively. The decolorization and COD removal of RO16 was determined using UV-Vis spectrophotometer (by the changes of absorption spectrum intensity of azo chromophore (-N=N-) at λ=388 and 492.50 nm and Hach spectrophotometer respectively. FTIR was used to determine functional groups present in the coconut trunk charcoal.

  3. Biological treatment of a textile effluent after electrochemical oxidation of reactive dyes.

    PubMed

    Vilaseca, Mercè; Gutiérrez, Maria-Carmen; López-Grimau, Victor; López-Mesas, Montserrat; Crespi, Martí

    2010-02-01

    In this work, a synthetic textile effluent containing a reactive dye (C.I. Reactive Orange 4) was treated in an electrochemical cell with titanium covered by platinum oxide (Ti/PtOx) electrodes to remove color. The discolored effluent was mixed with other textile mill process effluents (scouring, bleaching, washing, etc.), according to the rate of each effluent in the mill, and was submitted to biological treatment (activated sludge plant). Two biological plants were run simultaneously to evaluate the influence of oxidant products generated during the electrochemical treatment. The final chemical oxygen demand (COD) removal in both plants was 65 to 72%. The yield of the activated sludge plants was not affected by the addition of 10% of the discolored dyeing effluent (even when oxidants products were not removed), which indicates that the previous electrochemical treatment do not produce inhibition effects on the biological plant. However, in the case of direct addition of the discolored effluent, the biological treatment plant required a longer adaptation period. In addition, the electrolytic respirometry tests showed that all the biodegradable organic matter was removed, which implies that the yield in organic matter removal was the maximum possible for this type of treatment.

  4. Electrochemical oxidation of the poultry manure anaerobic digested effluents for enhancing pollutants removal by Chlorella vulgaris.

    PubMed

    Wang, Mengzi; Cao, Wei; Wu, Yu; Lu, Haifeng; Li, Baoming

    2016-01-01

    The mechanisms and pseudo-kinetics of the electrochemical oxidation for wastewater treatment and the synergistic effect of combining algal biological treatment were investigated. NaCl, Na2SO4 and HCl were applied to compare the effect of electrolyte species on nutrients removal. NaCl was proved to be more efficient in removing ammonia ([Formula: see text]), total phosphorus (TP), total organic carbon (TOC) and inorganic carbon (IC). [Formula: see text] oxidation by using Ti/Pt-IrO2 electrodes was modelled, which indicates that the [Formula: see text] removal followed the zero-order kinetic with sufficient Cl(-) and the first-order kinetic with insufficient Cl(-), respectively. The feasibility of combining electrochemical oxidation with microalgae cultivation for wastewater treatment was also determined. A 2 h electrochemical pretreatment reduced 57% [Formula: see text], 76% TP, 72% TOC and 77% IC from the digested effluent, which is applied as feedstock for algae cultivation, and resulted in increasing both the biomass production and pollutants removal efficiencies of the algal biological process.

  5. Simultaneous hydrogen production and electrochemical oxidation of organics using boron-doped diamond electrodes.

    PubMed

    Jiang, Juyuan; Chang, Ming; Pan, Peng

    2008-04-15

    This paper presents advantages of using a boron-doped diamond (BDD) electrode for hydrogen production and wastewater treatment in a single electrochemical cell. Results indicated that the BDD electrode possessed the widest known electrochemical window, allowing new possibilities for both anodic and cathodic reactions to simultaneously take place. The BDD electrode exhibited high anodic potential, generating high oxidation state radicals that facilitated oxidation of toxic waste organic compounds such as 4-nitrophenols. In contrast, because of widening of potential windows, the rate of hydrogen evolution at the cathode was significantly increased. Time-on-stream concentrations of reaction intermediates were monitored to elucidate mechanism involved in 4-nitrophenol oxidation. Spalling, fouling, or reduction in the thickness of thin-film diamond coating was not observed. Overall, the BDD electrode exhibits unique properties including chemical inertness, anticorrosion, and extended service life. These properties are especially important in wastewater treatment. Economic advantages were attributed to the low cost and long duration BDD electrode and the valuable hydrogen byproduct produced. Analysis has shown that technology associated with the BDD electrode could be effectively implemented with minimum energy input and capital requirements. When combined with solar energy and fuel cells, electrochemical wastewater processing can become energy efficient and cost-effective.

  6. A Zinc Oxide Nanoflower-Based Electrochemical Sensor for Trace Detection of Sunset Yellow

    PubMed Central

    Ya, Yu; Jiang, Cuiwen; Li, Tao; Liao, Jie; Fan, Yegeng; Wei, Yuning; Yan, Feiyan; Xie, Liping

    2017-01-01

    Zinc oxide nanoflower (ZnONF) was synthesized by a simple process and was used to construct a highly sensitive electrochemical sensor for the detection of sunset yellow (SY). Due to the large surface area and high accumulation efficiency of ZnONF, the ZnONF-modified carbon paste electrode (ZnONF/CPE) showed a strong enhancement effect on the electrochemical oxidation of SY. The electrochemical behaviors of SY were investigated using voltammetry with the ZnONF-based sensor. The optimized parameters included the amount of ZnONF, the accumulation time, and the pH value. Under optimal conditions, the oxidation peak current was linearly proportional to SY concentration in the range of 0.50–10 μg/L and 10–70 μg/L, while the detection limit was 0.10 μg/L (signal-to-noise ratio = 3). The proposed method was used to determine the amount of SY in soft drinks with recoveries of 97.5%–103%, and the results were in good agreement with the results obtained by high-performance liquid chromatography. PMID:28282900

  7. Electrochemical regeneration of a reduced graphene oxide/magnetite composite adsorbent loaded with methylene blue.

    PubMed

    Sharif, Farbod; Gagnon, Luke R; Mulmi, Suresh; Roberts, Edward P L

    2017-05-01

    In this work, two different reduced graphene oxide/iron oxide (rGO-IO) nanocomposites with different iron oxide loadings were fabricated using a one-step solvothermal method. The structure, properties and applications of the synthesized nanocomposites were evaluated with Raman spectroscopy, attenuated total reflectance Fourier transform infrared spectroscopy, thermogravimetric analysis, X-ray diffraction, electron microscopy, and energy-dispersive X-ray spectroscopy. The iron oxide is in the form of magnetite (Fe3O4), so that the resultant adsorbent can readily be separated from the treated water using a magnetic field. The ability of the nanocomposites to remove methylene blue (MB) from water by adsorption was investigated. The highest adsorptive capacity observed was 39 mg g(-1), for the composite containing 60 wt% iron oxide. The adsorptive capacity of the rGO-IO decreased to 26 mg g(-1) when the mass fraction of iron oxide was increased to 75 wt%. Electrochemical regeneration of MB loaded rGO-IO was also investigated. The electrochemical regeneration was found to be rapid and with low electrical energy consumption relative to conventional adsorbents, due to the high electrical conductivity and nonporous surface of the rGO. A regeneration efficiency of 100% was obtained after 30 min of electrochemical treatment using a 2 mm thick bed of rGO-IO loaded with 39 mg g(-1) MB, using a current density of 10 mA cm(-2). Multiple adsorption-electrochemical regeneration cycles demonstrated that the surface of the rGO was modified leading to increase in the adsorptive capacity to around 80 mg g(-1) after the second regeneration cycle. The morphology of the rGO was observed to change significantly after electrochemical regeneration, suggesting that the rGO based adsorbent materials could only be used for a few cycles. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Preparation of In X (X = P, As, Sb) thin films by electrochemical methods

    SciTech Connect

    Ortega, J.; Herrero, J. )

    1989-11-01

    Compounds of the III-V semiconductor family are widely used as photovoltaic detectors, optical recording materials, in semiconductor super lattice structures, etc. Also, many stable compounds of the group of semiconductor materials have been proposed as candidates for efficient solar energy conversion in solid-state photovoltaic or photoelectrochemical devices, where GaAs and InP present the most impressive solar conversion performance and stability. As III-V compound semiconductor device technology is advanced, it becomes desirable to apply some of the electrochemical preparation and characterization techniques which have proven useful for the preparation of II-VI semiconductors. While photoelectrochemical techniques have been used to characterize III-V semiconductors, few details have been published about their electrochemical preparation. GaP, InP, and GaAs have been electrodeposited from fused salt. In-Sb alloys have been deposited from a variety of electrolytes, but there is little information on electrodeposition of In-As compounds. The authors have demonstrated previously that it is possible to obtain In{sub 2}Se{sub 3} and In{sub 2}S{sub 3} from electroplated metallic indium films by solid-phase or gas-phase chalcogenization at high temperatures. In this paper they present results on both the electrodeposition of In-Sb and In-As alloys that can be converted to crystalline, well-defined phases of InSb and InAs, and also on the formation of InP thin films by a phosphorization treatme

  9. Two-step electrochemical synthesis of polypyrrole/reduced graphene oxide composites as efficient Pt-free counter electrode for plastic dye-sensitized solar cells.

    PubMed

    Liu, Wantao; Fang, Yanyan; Xu, Peng; Lin, Yuan; Yin, Xiong; Tang, Guangshi; He, Meng

    2014-09-24

    Polypyrrole/reduced graphene oxide (PPy/RGO) composites on the rigid and plastic conducting substrates were fabricated via a facile two-step electrochemical process at low temperature. The polypyrrole/graphene oxide (PPy/GO) composites were first prepared on the substrate with electrochemical polymerization method, and the PPy/RGO composites were subsequently obtained by electrochemically reducing the PPy/GO. The resultant PPy/GO and PPy/RGO composites were porous, in contrast to the dense and flat pristine PPy films. The cyclic voltammetry measurement revealed that resultant composites exhibited a superior catalytic performance for triiodide reduction in the order of PPy/RGO > PPy/GO > PPy. The catalytic activity of PPy/RGO was comparable to that of Pt counter electrode (CE). Under the optimal conditions, an energy conversion efficiency of 6.45% was obtained for a rigid PPy/RGO-based dye-sensitized solar cell, which is 90% of that for a thermally deposited Pt-based device (7.14%). A plastic counter electrode was fabricated by depositing PPy/RGO composites on the plastic ITO/PEN substrate, and then an all-plastic device was assembled and exhibited an energy conversion efficiency of 4.25%, comparable to that of the counterpart using a sputtered-Pt CE (4.83%) on a plastic substrate. These results demonstrated that electrochemical synthesis is a facile low-temperature method to fabricate high-performance RGO/polymer composite-based CEs for plastic DSCs.

  10. Electrochemical degradation of polycyclic aromatic hydrocarbons in creosote solution using ruthenium oxide on titanium expanded mesh anode.

    PubMed

    Tran, Lan-Huong; Drogui, Patrick; Mercier, Guy; Blais, Jean-François

    2009-05-30

    In this study, expanded titanium (Ti) covered with ruthenium oxide (RuO(2)) electrode was used to anodically oxidize polycyclic aromatic hydrocarbons (PAH) in creosote solution. Synthetic creosote-oily solution (COS) was prepared with distilled water and a commercial creosote solution in the presence of an amphoteric surfactant; Cocamidopropylhydroxysultaine (CAS). Electrolysis was carried out using a parallelepipedic electrolytic 1.5-L cell containing five anodes (Ti/RuO(2)) and five cathodes (stainless steel, 316 L) alternated in the electrode pack. The effects of initial pH, temperature, retention time, supporting electrolyte, current density and initial PAH concentration on the process performance were examined. Experimental results revealed that a current density of 9.23 mA cm(-2) was beneficial for PAH oxidation. The sum of PAH concentrations for 16 PAHs could be optimally diminished up to 80-82% while imposing a residence time in the electrolysis cell of 90 min. There was not a significant effect of the electrolyte (Na(2)SO(4)) concentration on oxidation efficiency in the investigated range of 500-4000 mg/L. However, an addition of 500 mg Na(2)SO(4)L(-1) was required to reduce the energy consumption and the treatment cost. Besides, there was no effect of initial PAH concentration on oxidation efficiency in the investigated range of 270-540 mg PAHL(-1). Alkaline media was not favourable for PAH oxidation, whereas high performance of PAH degradation could be recorded without initial pH adjustment (original pH around 6.0). Likewise, under optimal conditions, 84% of petroleum hydrocarbon (C(10)-C(50)) was removed, whereas removal yields of 69% and 62% have been measured for O&G and COD, respectively. Microtox and Daphnia biotests showed that electrochemical oxidation using Ti/RuO(2) could be efficiently used to reduce more than 90% of the COS toxicity.

  11. Electrodeposition and electrochemical reduction of epitaxial metal oxide thin films and superlattices

    NASA Astrophysics Data System (ADS)

    He, Zhen

    The focus of this dissertation is the electrodeposition and electrochemical reduction of epitaxial metal oxide thin films and superlattices. The electrochemical reduction of metal oxides to metals has been studied for decades as an alternative to pyrometallurgical processes for the metallurgy industry. However, the previous work was conducted on bulk polycrystalline metal oxides. Paper I in this dissertation shows that epitaxial face-centered cubic magnetite (Fe3O4 ) thin films can be electrochemically reduced to epitaxial body-centered cubic iron (Fe) thin films in aqueous solution on single-crystalline Au substrates at room temperature. This technique opens new possibilities to produce special epitaxial metal/metal oxide heterojunctions and a wide range of epitaxial metallic alloy films from the corresponding mixed metal oxides. Electrodeposition, like biomineralization, is a soft solution processing method which can produce functional materials with special properties onto conducting or semiconducting solid surfaces. Paper II in this dissertation presents the electrodeposition of cobalt-substituted magnetite (CoxFe3-xO4, 0 of cobalt-substituted magnetite (CoxFe3-xO4, 0oxide (Co3O4) thin films on stainless steel and Au single-crystalline substrates. The crystalline Co3O4 thin films exhibit high catalytic activity towards the oxygen evolution reaction in an alkaline solution. A possible application of the electrodeposited Co 3O4 is the fabrication of highly active and low-cost photoanodes for photoelectrochemical water-splitting cells.

  12. Electrochemical oxidation and protein adduct formation of aniline: a liquid chromatography/mass spectrometry study.

    PubMed

    Melles, Daniel; Vielhaber, Torsten; Baumann, Anne; Zazzeroni, Raniero; Karst, Uwe

    2012-04-01

    Historically, skin sensitization tests are typically based on in vivo animal tests. However, for substances used in cosmetic products, these tests have to be replaced according to the European Commission regulation no. 1223/2009. Modification of skin proteins by electrophilic chemicals is a key process associated with the induction of skin sensitization. The present study investigates the capabilities of a purely instrumental setup to determine the potential of commonly used non-electrophilic chemicals to cause skin sensitization by the generation of electrophilic species from the parent compound. In this work, the electrophiles were generated by the electrochemical oxidation of aniline, a basic industrial chemical which may also be released from azo dyes in cosmetics. The compound is a known sensitizer and was oxidized in an electrochemical thin-layer cell which was coupled online to electrospray ionization-mass spectrometry. The electrochemical oxidation was performed on a boron-doped diamond working electrode, which is able to generate hydroxyl radicals in aqueous solutions at high potentials. Without any pretreatment, the oxidation products were identified by electrospray ionization/time-of-flight mass spectrometry (ESI-ToF-MS) using their exact masses. A mass voltammogram was generated by plotting the obtained mass spectra against the applied potential. Oligomerization states with up to six monomeric units in different redox states of aniline were observed using this setup. This approach was extended to generate adducts between the oxidation products of aniline and the tripeptide glutathione. Two adducts were identified with this trapping experiment. Protein modification was carried out subsequently: Aniline was oxidized at a constant potential and was allowed to react with β-lactoglobulin A (β-LGA) or human serum albumin (HSA), respectively. The generated adducts were analyzed by liquid chromatography coupled to ESI-ToF-MS. For both β-LGA and HSA, aniline

  13. Electrochemical preparation of standard solutions of Pb(II) ions in ionic liquid for analysis of hydrophobic samples: The olive oil case.

    PubMed

    Baldo, M Antonietta; Stortini, Angela M; Moretto, Ligia M; Ongaro, Michael; Roman, Marco; Ugo, Paolo

    2017-09-01

    In this paper we present an electrochemical approach to prepare standard solutions of metal ions in a room temperature ionic liquid (IL), which can find useful application for analysis in hydrophobic matrices. The method, developed here for the case of lead ions, is based on the galvanostatic dissolution of a lead anode dipped directly in a suitable IL, namely tri-hexyl(tetradecyl)phosphonium bis (trifluoromethylsulfonyl) imide ([P14,6,6,6](+)[NTf2](-)). After each oxidation step, the metal dissolution process in the IL solutions was monitored by cyclic voltammetric measurements at a glassy carbon disk electrode. The results indicated that the peak current relevant to the reduction of the electro-generated Pb(II) increased linearly while increasing the oxidation time. By varying the oxidation time from 200 to 6000s, a set of Pb((II))/[P14,6,6,6](+)[NTf2](-) solutions at concentrations ranging between 10 and 300μgg(-1) was prepared. To validate the efficiency of the electrochemical procedure to produce metal ion standard solutions, the Pb content was quantified by developing a microwave digestion procedure specifically suitable for the IL medium, followed by ICP-QMS analysis in the digested standards. The results indicated a satisfactory agreement between concentrations found by ICP-QMS and calculated from electrochemical data, with a coulometric efficiency of Pb(II) generation in ionic liquid ≥95.6%. Finally, the applicability of the Pb((II))/IL solutions as standards for analyses in hydrophobic media was tested by determining, by ICP-QMS, the Pb content in an extra-virgin olive oil spiked with known amounts of a Pb((II))/IL standard. Satisfactory Pb recoveries, ≥96%, were measured. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Preparation and quality control of silver nanoparticle-antibody conjugate for use in electrochemical immunoassays.

    PubMed

    Szymanski, Mateusz S; Porter, Robert A

    2013-01-31

    Metal nanoparticle-antibody conjugates are often used as optical or electrochemical markers in applications like immunohistochemistry, lateral flow tests, biosensors and immunoassays. In order to serve that role, an antibody needs to be immobilized on the surface of the nanoparticle. This is easily done, as proteins bind to gold and silver nanoparticles spontaneously. However, this immobilization process might result in nanoparticle aggregation or the loss of the bioactivity of the conjugated antibodies. In this work the optimization of antibody immobilization on silver colloid in order to obtain conjugates with the best possible activity is investigated. The parameters investigated were the type of immobilization buffer, its molarity and pH, the nanoparticle/antibody ratio and also blocking and washing protocols to reduce non-specific binding. The functionality of the obtained conjugates was tested with electrochemical immunoassay. It was found out that the optimum environment for immobilization of an anti-myoglobin antibody on silver nanoparticles was 0.2M boric acid pH 6.5 with 10 μg of antibody loading per 1 mL of silver colloid. For an anti-troponin antibody it was 0.1M boric acid pH 7.5 also with 10 μg/mL of antibody loading. The main problem for silver conjugation was the tendency of silver nanoparticles to aggregate during the immobilization process, but by choosing the optimum conditions the aggregation problem was completely removed. Here it is demonstrated that by using the conjugates prepared with an optimized protocol an increase in the sensitivity of the assay 10 times can be achieved. The electrochemical immunoassay described here can be used as a test for quality control of conjugates and for the estimation of batch-to-batch variability. Copyright © 2012 Elsevier B.V. All rights reserved.

  15. Electrochemical synthesis of tetragonal oxide tungsten bronze nanofilms on platinum

    NASA Astrophysics Data System (ADS)

    Kosov, A. V.; Semerikova, O. L.; Vakarin, S. V.; Pankratov, A. A.; Plaksin, S. V.; Korzun, I. V.; Akashev, L. A.; Zaykov, Yu. P.

    2017-02-01

    We are the first to synthesize nanofilms of tetragonal oxide tungsten bronze (OTB) on a Pt(110) substrate by the electrolysis of the K2WO4-Na2WO4-WO3 melt at 700 and 750°C. The composition and the morphology of OTB are shown to depend on the deposition potential and the WO3 concentration in the melt. The laws of formation of tetragonal OTB films are discussed. The synthesized OTB samples are found to have a good thermal stability in the temperature range 20-800°C.

  16. Measurement of oxidized and methylated DNA bases by HPLC with electrochemical detection.

    PubMed

    Kaur, H; Halliwell, B

    1996-08-15

    Oxidative DNA damage is thought to be an important contributor to cancer development and to be affected by dietary constituents, so its accurate measurement is important. DNA methylation is recognized as an important mechanism affecting gene expression. In the present paper we describe an HPLC-with-electrochemical-detection procedure that allows rapid and sensitive measurement of four oxidized (2,6-diamino-4-hydroxy-5-formamidopyrimidine, 5-hydroxyuracil, 8-hydroxyguanine, 8-hydroxyadenine) and three methylated (7-methylguanine, 1-methylguanine, O6-methylguanine) bases in acid hydrolysates of DNA. Guanine was also detected, but was clearly separated from the other bases.

  17. Electrochemically-Controlled Compositional Oscillations of Oxide Surfaces

    SciTech Connect

    Mutoro, Eva; Crumlin, Ethan; Pöpke, Hendrik; Luerssen, Bjoern; Amati, Matteo; Abyaneh, Majid; Biegalski, Michael D; Christen, Hans M; Gregoratti, Luca; Janek, Jürgen; Shao-Horn, Yang

    2012-01-01

    Perovskite oxides can exhibit a wide range of interesting characteristics such as being catalytically active and electronically and/or ionically conducting, and thus they have been used in a number of solid-state devices such as solid oxide fuel cells and sensors. As the surface compositions of perovskites can greatly influence the catalytic properties, knowing and controlling their surface chemistries is crucial to enhance device performance. In this study, we demonstrate that the surface strontium (Sr) and cobalt (Co) concentrations of perovskite-based thin films can be controlled reversibly at elevated temperatures by applying small electrical potential biases. The surface chemistry changes of La0.8Sr0.2CoO3 (LSC113), LaSrCoO4 (LSC214), and LSC214-decorated LSC113 films (LSC113/214) were investigated in situ by utilizing synchrotron-based X-ray photoelectron spectroscopy (XPS), where the largest changes of surface Sr was found for the LSC113/214 surface. These findings offer the potential of reversibly controlling the surface functionality of perovskites.

  18. A dual electrochemical sensor for nitrite and nitric oxide.

    PubMed

    Zen, J M; Kumar, A S; Wang, H F

    2000-12-01

    Nafion/lead-ruthenate pyrochlore chemically modified electrode (NPyCME) showed a remarkable dual sensing activity toward NO2- oxidation and NO reduction as demonstrated by cyclic voltammetry (CV), ac-impedance spectroscopy and flow injection analysis (FIA). The mechanistic parameters of current function, charge transfer resistance and exchange current for the NPyCME, GCE and Nafion-coated GCE were evaluated and compared. The disproportionation reaction of NIIIO2- into NIVO3- + NIIO in acidic solution was used as a model system for testing the dual sensing ability of the NPyCME. The obtained crossover peak response for NO2- oxidation and NO reduction in pH 1.65 buffer solution gave the direct proof for the applicability of the NPyCME in the dual electrocatalytic action. By flow injection analysis, under optimized conditions, the calibration curve was linear in the range of 100 nM-100 microM and 800 nM-63.3 microM and the detection limit (S/N = 3) was 4.8 nM and 15.6 nM for NO2- and NO, respectively.

  19. Cobalt Oxide Nanoflowers for Electrochemical Determination of Glucose

    NASA Astrophysics Data System (ADS)

    Balouch, Quratulain; Ibupoto, Zafar Hussain; Khaskheli, Ghulam Qadir; Soomro, Razium Ali; Sirajuddin; Samoon, Muhammad Kashif; Deewani, Vinod Kumar

    2015-10-01

    This study reports a simple, economic, and efficient approach for synthesis of cobalt oxide (Co3O4) nanostructures by a low-temperature aqueous chemical growth method. The synthesized Co3O4 nanostructures were characterized by various techniques such as x-ray diffraction, x-ray photoelectron spectroscopy, and scanning electron microscopy. The synthesized nanostructures exhibited flower-shaped morphology with thickness of each pellet in the range of 200 to 300 nm. The synthesized Co3O4 nanostructures with excellent structural features exhibited high electrocatalytic activity towards the oxidation of glucose in alkaline solution. This enabled development of a highly sensitive (1618.71 µA mM-1 cm-2), stable and reproducible non-enzymatic glucose sensor. The developed sensor demonstrated high anti-interference capability against common interferents such as dopamine, ascorbic acid and uric acid. Furthermore, the applicability of the developed sensor for the determination of glucose from human blood serum provides an alternative approach for the routine glucose analysis.

  20. Writable electrochemical energy source based on graphene oxide.

    PubMed

    Wei, Di

    2015-10-14

    Graphene oxide (GO) was mainly used as raw material for various types of reduced graphene oxide (rGO) as a cost effective method to make graphene like materials. However, applications of its own unique properties such as extraordinary proton conductivity and super-permeability to water were overlooked. Here GO based battery-like planar energy source was demonstrated on arbitrary insulating substrate (e.g. polymer sheet/paper) by coating PEDOT, GO ink and rGO on Ag charge collectors. Energy from such GO battery depends on its length and one unit cell with length of 0.5 cm can generate energy capacity of 30 Ah/L with voltage up to 0.7 V when room temperature ionic liquid (RTIL) is added. With power density up to 0.4 W/cm(3) and energy density of 4 Wh/L, GO battery was demonstrated to drive an electrochromic device. This work is the first attempt to generate decent energy using the fast transported water molecules inside GO. It provides very safe energy source that enables new applications otherwise traditional battery technology can not make including building a foldable energy source on paper and platform for futuristic wearable electronics. A disposable energy source made of GO was also written on a plastic glove to demonstrate wearability.

  1. Writable electrochemical energy source based on graphene oxide

    PubMed Central

    Wei, Di

    2015-01-01

    Graphene oxide (GO) was mainly used as raw material for various types of reduced graphene oxide (rGO) as a cost effective method to make graphene like materials. However, applications of its own unique properties such as extraordinary proton conductivity and super-permeability to water were overlooked. Here GO based battery-like planar energy source was demonstrated on arbitrary insulating substrate (e.g. polymer sheet/paper) by coating PEDOT, GO ink and rGO on Ag charge collectors. Energy from such GO battery depends on its length and one unit cell with length of 0.5 cm can generate energy capacity of 30 Ah/L with voltage up to 0.7 V when room temperature ionic liquid (RTIL) is added. With power density up to 0.4 W/cm3 and energy density of 4 Wh/L, GO battery was demonstrated to drive an electrochromic device. This work is the first attempt to generate decent energy using the fast transported water molecules inside GO. It provides very safe energy source that enables new applications otherwise traditional battery technology can not make including building a foldable energy source on paper and platform for futuristic wearable electronics. A disposable energy source made of GO was also written on a plastic glove to demonstrate wearability. PMID:26462557

  2. Writable electrochemical energy source based on graphene oxide

    NASA Astrophysics Data System (ADS)

    Wei, Di

    2015-10-01

    Graphene oxide (GO) was mainly used as raw material for various types of reduced graphene oxide (rGO) as a cost effective method to make graphene like materials. However, applications of its own unique properties such as extraordinary proton conductivity and super-permeability to water were overlooked. Here GO based battery-like planar energy source was demonstrated on arbitrary insulating substrate (e.g. polymer sheet/paper) by coating PEDOT, GO ink and rGO on Ag charge collectors. Energy from such GO battery depends on its length and one unit cell with length of 0.5 cm can generate energy capacity of 30 Ah/L with voltage up to 0.7 V when room temperature ionic liquid (RTIL) is added. With power density up to 0.4 W/cm3 and energy density of 4 Wh/L, GO battery was demonstrated to drive an electrochromic device. This work is the first attempt to generate decent energy using the fast transported water molecules inside GO. It provides very safe energy source that enables new applications otherwise traditional battery technology can not make including building a foldable energy source on paper and platform for futuristic wearable electronics. A disposable energy source made of GO was also written on a plastic glove to demonstrate wearability.

  3. High-temperature "spectrochronopotentiometry": correlating electrochemical performance with in situ Raman spectroscopy in solid oxide fuel cells.

    PubMed

    Kirtley, John D; Halat, David M; McIntyre, Melissa D; Eigenbrodt, Bryan C; Walker, Robert A

    2012-11-20

    Carbon formation or "coking" on solid oxide fuel cell (SOFC) anodes adversely affects performance by blocking catalytic sites and reducing electrochemical activity. Quantifying these effects, however, often requires correlating changes in SOFC electrochemical efficiency measured during operation with results from ex situ measurements performed after the SOFC has been cooled and disassembled. Experiments presented in this work couple vibrational Raman spectroscopy with chronopotentiometry to observe directly the relationship between graphite deposited on nickel cermet anodes and the electrochemical performance of SOFCs operating at 725 °C. Raman spectra from Ni cermet anodes at open circuit voltage exposed to methane show a strong vibrational band at 1556 cm(-1) assigned to the "G" mode of highly ordered graphite. When polarized in the absence of a gas-phase fuel, these carbon-loaded anodes operate stably, oxidizing graphite to form CO and CO(2). Disappearance of graphite intensity measured in the Raman spectra is accompanied by a steep ∼0.8 V rise in the cell potential needed to keep the SOFC operating under constant current conditions. Continued operation leads to spectroscopically observable Ni oxidation and another steep rise in cell potential. Time-dependent spectroscopic and electrochemical measurements pass through correlated equivalence points providing unequivocal, in situ evidence that identifies how SOFC performance depends on the chemical condition of its anode. Chronopotentiometric data are used to quantify the oxide flux necessary to eliminate the carbon initially present on the SOFC anode, and data show that the oxidation mechanisms responsible for graphite removal correlate directly with the electrochemical condition of the anode as evidenced by voltammetry and impedance measurements. Electrochemically oxidizing the Ni anode damages the SOFC significantly and irreversibly. Anodes that have been reconstituted following electrochemical oxidation of

  4. Electrochemical oxidation of oxalic acid at highly boron-doped diamond electrodes.

    PubMed

    Ivandini, Tribidasari A; Rao, Tata N; Fujishima, Akira; Einaga, Yasuaki

    2006-05-15

    Electrochemical oxidation of oxalic acid has been investigated at bare, highly boron-doped diamond electrodes. Cyclic voltammetry and flow injection analysis with amperometric detection were used to study the electrochemical reaction. Hydrogen-terminated diamonds exhibited well-defined peaks of oxalic acid oxidation in a wide pH range. A good linear response was observed for a concentration range from 50 nM to 10 microM, with an estimated detection limit of approximately 0.5 nM (S/N = 3). In contrast, oxygen-terminated diamonds showed no response for oxalic acid oxidation inside the potential window, indicating that surface termination contributed highly to the control of the oxidation reaction. An investigation with glassy carbon electrodes was conducted to confirm the surface termination effect on oxalic acid oxidation. Although a hydrogen-terminated glassy carbon electrode showed an enhancement of signal-to-background ratio in comparison with untreated glassy carbon, less stability of the current responses was observed than that at hydrogen-terminated diamond.

  5. Conductive diamond electrochemical oxidation of caffeine-intensified biologically treated urban wastewater.

    PubMed

    Martín de Vidales, María J; Millán, María; Sáez, Cristina; Pérez, José F; Rodrigo, Manuel A; Cañizares, Pablo

    2015-10-01

    In this work, the usefulness of Conductive Diamond Electrochemical Oxidation (CDEO) to degrade caffeine in real urban wastewater matrixes was assessed. The oxidation of actual wastewater intensified with caffeine (from 1 to 100 mg L(-1)) was studied, paying particular attention to the influence of the initial load of caffeine and the differences observed during the treatment of caffeine in synthetic wastewater. The results showed that CDEO is a technology that is capable of efficiently degrading this compound even at very low concentrations and that it can even be completely depleted. Profiles of the ionic species of S (SO4(2-)), N (NH4(+), NO3(-)) and Cl (ClO(-), ClO3(-) and ClO4(-)) were monitored and explained for plausible oxidation mechanisms. It was observed that the efficiency achieved is higher in the treatment of real wastewater than in the oxidation of synthetic wastewater because of the contribution of electrogenerated oxidant species such as hypochlorite. The formation of chlorate and perchlorate during electrochemical processes was observed, and a combined strategy to prevent this important drawback was successfully tested based on the application of low current densities with the simultaneous dosing of hydrogen peroxide. Copyright © 2015 Elsevier Ltd. All rights reserved.

  6. Formation and electrochemical characterization of anodic ZrO2-WO3 mixed oxide nanotubular arrays

    NASA Astrophysics Data System (ADS)

    Whitman, Stuart R.; Raja, Krishnan S.

    2014-06-01

    ZrO2-WO3 mixed oxide nanotubes were synthesized by a simple electrochemical anodization route. The oxide nanotubes contained a mixture of metastable hexagonal WO3 and monoclinic (and orthorhombic) ZrO2 phases, as well as a mixed-oxide ZrW2O8 phase that showed a metastable tetragonal symmetry. Evaluation of photo-activity of the materials showed generation of photo-potentials of -85 mV and -230 mV in the as-anodized and annealed conditions. Because of the mismatch in the band edge positions of the WO3 and ZrO2 phases and the resultant relaxation of photo-generated charge carriers, no significant photo-current density could be observed. The arrays of oxide nanotubes are considered for electrochemical capacitor application because of their morphology-assisted fast charge/discharge kinetics and large surface area. Presence of a large concentration of charge defects (on the order of 1021 cm-3) and the reported high proton conductivity of the ZrO2-WO3 mixed oxide rendered high capacitance, which decreased with an increase in the scan rate of cyclic voltammetry. The highest measured capacitance was 40.03 mF/cm2 at a scan rate of 10 mV/s and the lowest was 1.93 mF/cm2 at 1 V/s in 1 M sulfuric acid solution.

  7. Direct electrochemical reduction of solid uranium oxide in molten fluoride salts

    NASA Astrophysics Data System (ADS)

    Gibilaro, Mathieu; Cassayre, Laurent; Lemoine, Olivier; Massot, Laurent; Dugne, Olivier; Malmbeck, Rikard; Chamelot, Pierre

    2011-07-01

    The direct electrochemical reduction of UO 2 solid pellets was carried out in LiF-CaF 2 (+2 mass.% Li 2O) at 850 °C. An inert gold anode was used instead of the usual reactive sacrificial carbon anode. In this case, oxidation of oxide ions present in the melt yields O 2 gas evolution on the anode. Electrochemical characterisations of UO 2 pellets were performed by linear sweep voltammetry at 10 mV/s and reduction waves associated to oxide direct reduction were observed at a potential 150 mV more positive in comparison to the solvent reduction. Subsequent, galvanostatic electrolyses runs were carried out and products were characterised by SEM-EDX, EPMA/WDS, XRD and microhardness measurements. In one of the runs, uranium oxide was partially reduced and three phases were observed: nonreduced UO 2 in the centre, pure metallic uranium on the external layer and an intermediate phase representing the initial stage of reduction taking place at the grain boundaries. In another run, the UO 2 sample was fully reduced. Due to oxygen removal, the U matrix had a typical coral-like structure which is characteristic of the pattern observed after the electroreduction of solid oxides.

  8. Surface functionalization of fluorine-doped tin oxide samples through electrochemical grafting.

    PubMed

    Lamberti, F; Agnoli, S; Brigo, L; Granozzi, G; Giomo, M; Elvassore, N

    2013-12-26

    Transparent conductive oxides are emerging materials in several fields, such as photovoltaics, photoelectrochemistry, and optical biosensing. Their high chemical inertia, which ensured long-term stability on one side, makes challenging the surface modification of transparent conductive oxides; long-term robust modification, high yields, and selective surface modifications are essential prerequisite for any further developments. In this work, we aim at inducing chemical functionality on fluorine-doped tin oxide surfaces (one of the most inexpensive transparent conductive oxide) by means of electrochemical grafting of aryl diazonium cations. The grafted layers are fully characterized by photoemission spectroscopy, cyclic voltammetry, and atomic force microscopy showing linear correlation between surface coverage and degree of modification. The electrochemical barrier effect of modified surfaces was studied at different pH to characterize the chemical nature of the coating. We showed immuno recognition of biotin complex built onto grafted fluorine-doped tin oxides, which opens the perspective of integrating FTO samples with biological-based devices.

  9. Preparation of Cu-Ni/YSZ solid oxide fuel cell anodes using microwave irradiation

    NASA Astrophysics Data System (ADS)

    Islam, Shamiul; Hill, Josephine M.

    A microwave irradiation process is used to deposit Cu nanoparticles on the Ni/YSZ anode of an electrolyte-supported solid oxide fuel cell (SOFC). The reaction time in the microwave is only 15 s for the deposition of 6 wt% Cu (with respect to Ni) from a solution of Cu(NO 3) 2·3H 2O and ethylene glycol (HOCH 2CH 2OH). The morphology of the deposited Cu particles is spherical and the average size of the particles is less than 100 nm. The electrochemical performance of the microwave Cu-coated Ni/YSZ anodes is tested in dry H 2 and dry CH 4 at 1073 K, and the anodes are characterized with scanning electron microscopy, electrochemical impedance spectroscopy, and temperature-programmed oxidation. The results indicate that preparation of the anodes by the microwave technique produces similar performance trend as those reported for Cu-Ni/YSZ/CeO 2 anodes prepared by impregnation. Specifically, less carbon is formed on the Cu-Ni/YSZ than on conventional Ni/YSZ anodes when exposed to dry methane and the carbon that does form is more reactive.

  10. Preparation and electrochemical properties of carbon-coated LiFePO4 hollow nanofibers

    NASA Astrophysics Data System (ADS)

    Wei, Bin-bin; Wu, Yan-bo; Yu, Fang-yuan; Zhou, Ya-nan

    2016-04-01

    Carbon-coated LiFePO4 hollow nanofibers as cathode materials for Li-ion batteries were obtained by coaxial electrospinning. X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Brunauer-Emmett-Teller specific surface area analysis, galvanostatic charge-discharge, and electrochemical impedance spectroscopy (EIS) were employed to investigate the crystalline structure, morphology, and electrochemical performance of the as-prepared hollow nanofibers. The results indicate that the carbon-coated LiFePO4 hollow nanofibers have good long-term cycling performance and good rate capability: at a current density of 0.2C (1.0C = 170 mA·g-1) in the voltage range of 2.5-4.2 V, the cathode materials achieve an initial discharge specific capacity of 153.16 mAh·g-1 with a first charge-discharge coulombic efficiency of more than 97%, as well as a high capacity retention of 99% after 10 cycles; moreover, the materials can retain a specific capacity of 135.68 mAh·g-1, even at 2C.

  11. [An investigation of HAP/organic polymer composite coatings prepared by electrochemical co-deposition technique].

    PubMed

    Hu, Haobing; Lin, Changjian; Leng, Yang

    2003-03-01

    An electrochemical co-deposition technique has been developed to prepare a hydroxyapatite (HAP)/organic polymer composite coatings on Ti surface as new biomaterial of hard tissue. The composite coating of organic polymer and calcium phosphate is formed by adding a water soluble polymer of the ethylene series to NH4H2PO4-Ca (NO3)2 solution when conducting an appropriate electrochemical co-deposition experiment. The XRD, SEM, XPS, SIMS and nano indent measurements were performed to characterize the morphology, composition, structure and surface stiffness of the composite coating. It was found that the morphology and surface hardness of the coatings showed a remarkable modification when introducing a minor polymer to HAP coating, and the bonding force between the coating and metal substrate was distinctly increased. The incorporation of minor organic polymer into the HAP compound at molecular level will improve the mechanical properties and morphology of the composite coatings, and this may be helpful to raising its bio-activity.

  12. In-Situ XPS Monitoring and Characterization of Electrochemically Prepared Au Nanoparticles in an Ionic Liquid

    PubMed Central

    2017-01-01

    Gold nanoparticles (Au NPs) have been electrochemically prepared in situ and in vacuo using two different electrochemical device configurations, containing an ionic liquid (IL), N-N-diethyl-N-methyl-N-(2-methoxyethyl)ammonium bis(trifluoromethanesulfonyl)imide, that serves both as reaction and as stabilizing media for the NPs. It was observed in both devices that Au NPs were created using an anodically triggered route. The created Au NPs are relatively small (3–7 nm) and reside within the IL medium. X-ray photoelectron spectroscopy is utilized to follow not only the formation of the NPs but also their charging/discharging properties, by monitoring the charging shifts of the Au4f peak representing the electrodes and also the Au NPs as well as the F1s peak of the IL after polarizing one of the electrodes. Accordingly, DC polarization across the electrodes leads to a uniform binding energy shift of F1s of the IL along with that of Au4f of the NPs within. Moreover, this shift corresponds to only half of the applied potential. AC polarization brings out another dimension for demonstrating further the harmony between the charging/discharging property of the IL medium and the Au NPs in temporally and laterally resolved fashions. Polarization of the electrodes result in perfect spectral separation of the Au4f peaks of the NPs from those of the metal in both static (DC) and in time- and position-dependent (AC) modes. PMID:28261688

  13. Preparation and electrochemical performance of gel polymer electrolytes using tri(ethylene glycol) dimethacrylate

    NASA Astrophysics Data System (ADS)

    Kim, Hyun-Soo; Shin, Jung-Han; Doh, Chil-Hoon; Moon, Seong-In; Kim, Sang-Pil

    A gel polymer electrolyte (GPE) is prepared from tri(ethylene glycol) dimethacrylate monomer, benzoyl peroxide, and 1.0 M LiPF 6/ethylene carbonate:diethyl carbonate (1:1 vol.%). The LiCoO 2|graphite cells are assembled and their electrochemical properties are evaluated at various current densities and temperatures. The viscosity of the precursor containing 5 vol.% tri(ethylene glycol) dimethacrylate monomer is around 4.6 mPa s. The ionic conductivity of the gel polymer electrolyte at 20 °C is around 5.9×10 -3 S cm -1. The gel polymer electrolyte has good electrochemical stability up to 4.5 V versus Li/Li +. The capacity of the cell at the 1.0 C rate is 89% of the discharge capacity at the 0.2 C rate. The capacity of the cell at temperature of -10 °C is 81% of the discharge capacity at 20 °C. The discharge capacity of the cell with gel polymer electrolyte is stable with charge-discharge cycling.

  14. α-Fe2O3 nanotubes-reduced graphene oxide composites as synergistic electrochemical capacitor materials

    NASA Astrophysics Data System (ADS)

    Lee, K. K.; Deng, S.; Fan, H. M.; Mhaisalkar, S.; Tan, H. R.; Tok, E. S.; Loh, K. P.; Chin, W. S.; Sow, C. H.

    2012-04-01

    We present a facile approach for the fabrication of a nanocomposite comprising α-Fe2O3 nanotubes (NTs) anchored on reduced graphene oxide (rGO) for electrochemical capacitors (ECs). The hollow tubular structure of the α-Fe2O3 NTs presents a high surface area for reaction, while the incorporation of rGO provides an efficient two-dimensional conductive pathway to allow fast, reversible redox reaction. As a result, the nanocomposite materials exhibit a specific capacitance which is remarkably higher (~7 times) than α-Fe2O3 NTs alone. In addition, the nanocomposites show excellent cycling life and large negative potential window. These findings suggest that such nanocomposites are a promising candidate as negative electrodes in asymmetrical capacitors with neutral electrolytes.We present a facile approach for the fabrication of a nanocomposite comprising α-Fe2O3 nanotubes (NTs) anchored on reduced graphene oxide (rGO) for electrochemical capacitors (ECs). The hollow tubular structure of the α-Fe2O3 NTs presents a high surface area for reaction, while the incorporation of rGO provides an efficient two-dimensional conductive pathway to allow fast, reversible redox reaction. As a result, the nanocomposite materials exhibit a specific capacitance which is remarkably higher (~7 times) than α-Fe2O3 NTs alone. In addition, the nanocomposites show excellent cycling life and large negative potential window. These findings suggest that such nanocomposites are a promising candidate as negative electrodes in asymmetrical capacitors with neutral electrolytes. Electronic supplementary information (ESI) available: Summary of electrochemical properties of various metal oxide-graphene materials composite electrodes (Table S1); experimental procedures, UV-Vis absorption spectra of GO and rGO (Fig. S1); X-ray photoemission spectra (XPS) of Fe2p (Fig. S2) and C1s (Fig. S3) core levels; percentage of various oxygenated functional groups from deconvolution of the C1s peak (Table S2

  15. Graphitic carbon nitride (g-C3N4) coated titanium oxide nanotube arrays with enhanced photo-electrochemical performance.

    PubMed

    Sun, Mingxuan; Fang, Yalin; Kong, Yuanyuan; Sun, Shanfu; Yu, Zhishui; Umar, Ahmad

    2016-08-09

    Herein, we report the successful formation of graphitic carbon nitride coated titanium oxide nanotube array thin films (g-C3N4/TiO2) via the facile thermal treatment of anodized Ti sheets over melamine. The proportion of C3N4 and TiO2 in the composite can be adjusted by changing the initial addition mass of melamine. The as-prepared samples are characterized by several techniques in order to understand the morphological, structural, compositional and optical properties. UV-vis absorption studies exhibit a remarkable red shift for the g-C3N4/TiO2 thin films as compared to the pristine TiO2 nanotubes. Importantly, the prepared composites exhibit an enhanced photocurrent and photo-potential under both UV-vis and visible light irradiation. Moreover, the observed maximum photo-conversion efficiency of the prepared composites is 1.59 times higher than that of the pristine TiO2 nanotubes. The optical and electrochemical impedance spectra analysis reveals that the better photo-electrochemical performance of the g-C3N4/TiO2 nanotubes is mainly due to the wider light absorption and reduced impedance compared to the bare TiO2 nanotube electrode. The presented work demonstrates a facile and simple method to fabricate g-C3N4/TiO2 nanotubes and clearly revealed that the introduction of g-C3N4 is a new and innovative approach to improve the photocurrent and photo-potential efficiencies of TiO2.

  16. Preparation of high-quality palladium nanocubes heavily deposited on nitrogen-doped graphene nanocomposites and their application for enhanced electrochemical sensing.

    PubMed

    Shen, Yu; Rao, Dejiang; Bai, Wushuang; Sheng, Qinglin; Zheng, Jianbin

    2017-04-01

    A nanocomposite of high-quality palladium nanocubes (PdNCs) decorated nitrogen-doped graphene (NGE/PdNC) was successfully prepared by using bromide ion as a capping agent and polyvinyl pyrrolidone as a stabilizer. The morphology and composition of NGE/PdNC nanocomposites were characterized by field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD) and Raman spectra. To explore the application of NGE/PdNC nanocomposites in electrochemistry, the electrocatalytic response to nitrite at a NGE/PdNC-based electrode was investigated. Thus, a highly sensitive and selective electrochemical sensor for the detection of nitrite was constructed based on a glassy carbon electrode modified with the NGE/PdNC nanocomposites. The electrochemical behavior of this nanocomposites was studied by electrochemical impedance spectroscopy, cyclic voltammetry and chronoamperometry. The electrochemical investigations proved that the NGE/PdNC nanocomposites exhibited good electrocatalytic performance for the oxidation of nitrite, including a wide linear range from 5.0×10(-7) to 1.51×10(-3)molL(-1), a high sensitivity of 342.4μAmM(-1)cm(-2) and a low detection limit of 0.11μmolL(-1) at the signal-to-noise ratio of 3 (S/N=3). This non-enzymatic sensor also showed a good reproducibility and stability. The obtained NGE/PdNC nanocomposites may be a potential composite for applying in the field of other electrochemical sensing, catalysis and optics.

  17. Boron-doped cobalt oxide thin films and its electrochemical properties

    NASA Astrophysics Data System (ADS)

    Kerli, S.

    2016-09-01

    The cobalt oxide and boron-doped cobalt oxide thin films were produced by spray deposition method. All films were obtained onto glass and fluorine-doped tin oxide (FTO) substrates at 400∘C and annealed at 550∘C. We present detailed analysis of the morphological and optical properties of films. XRD results show that boron doping disrupts the structure of the films. Morphologies of the films were investigated by using a scanning electron microscopy (SEM). Optical measurements indicate that the band gap energies of the films change with boron concentrations. The electrochemical supercapacitor performance test has been studied in aqueous 6 M KOH electrolyte and with scan rate of 5 mV/s. Measurements show that the largest capacitance is obtained for 3% boron-doped cobalt oxide film.

  18. Electrochemical oxidation of hydrazine and its derivatives on the surface of metal electrodes in alkaline media

    NASA Astrophysics Data System (ADS)

    Asazawa, Koichiro; Yamada, Koji; Tanaka, Hirohisa; Taniguchi, Masatoshi; Oguro, Keisuke

    Electrochemical oxidation of hydrazine and its derivatives on the surface of various metal electrodes in alkaline media was investigated. A comparison of various polycrystalline metal electrodes (Ni, Co, Fe, Cu, Ag, Au, and Pt) showed that Co and Ni electrodes have a lower onset potential for hydrazine oxidation than the Pt electrode. The onset oxidation potential of APA (aminopolyacrylamide), a hydrazine derivative (-0.127 V vs. reversible hydrogen electrode, RHE), was similar to that of hydrazine hydrate (-0.178 V vs. RHE) in the case of the Co electrode. APA oxidation was possible because of hydrazine desorption that was caused by APA hydrolysis. The hydrolysis reaction was brought about by a heat treatment. This result suggests that the hydrazine hydrolysis reaction of hydrazine derivatives makes it possible to store hydrazine hydrate safely.

  19. Mediated electrochemical oxidation of Rocky Flats combustible low level mixed wastes

    SciTech Connect

    Chiba, Z.

    1992-12-01

    Mediated Electrochemical Oxidation (MEO) was originally developed for dissolution of difficult to dissolve forms of plutonium oxide. It was also found to be effective for oxidizing non-polymerized organic materials. MEO is an inherently safe process since the hazardous and radioactive materials are completely contained in the aqueous phase, and operating temperatures and pressures of the system are low (well below 100 {degree}C and 30 psig). The most commonly used mediator-electrolyte combination is silver in nitric acid. The process produces divalent silver ion, a strong oxidizing agent, which dissolves the radioactive components of mixed wastes and destroys the organic components. In the past, work at LLNL has been focused on understanding the basic science and modeling the dissolution and destruction mechanisms. Reaction rates of water with Ag(H) were measured using spectrophotometric methods, and the diffusivity of silver ions in nitric acid was estimated using a rotating disk electrode.

  20. Electrochemical oxidation of 243Am(III) in nitric acid by a terpyridyl-derivatized electrode

    SciTech Connect

    Dares, C. J.; Lapides, A. M.; Mincher, B. J.; Meyer, T. J.

    2015-11-05

    A high surface area, tin-doped indium oxide electrode surface-derivatized with a terpyridine ligand has been applied to the oxidation of trivalent americium to Am(V) and Am(VI) in nitric acid. Potentials as low as 1.8 V vs. the saturated calomel electrode are used, 0.7 V lower than the 2.6 V potential for one-electron oxidation of Am(III) to Am(IV) in 1 M acid. This simple electrochemical procedure provides, for the first time, a method for accessing the higher oxidation states of Am in non-complexing media for developing the coordination chemistries of Am(V) and Am(VI) and, more importantly, for separation of americium from nuclear waste streams.

  1. An electrochemical approach to graphene oxide coated sulfur for long cycle life.

    PubMed

    Moon, Joonhee; Park, Jungjin; Jeon, Cheolho; Lee, Jouhahn; Jo, Insu; Yu, Seung-Ho; Cho, Sung-Pyo; Sung, Yung-Eun; Hong, Byung Hee

    2015-08-21

    Owing to the possibilities of achieving high theoretical energy density and gravimetric capacity, sulfur has been considered as a promising cathode material for rechargeable lithium batteries. However, sulfur shows rapid capacity fading due to the irreversible loss of soluble polysulfides and the decrease in active sites needed for conducting agents. Furthermore, the low electrical conductivity of sulfur hampers the full utilization of active materials. Here we report that graphene oxide coated sulfur composites (GO-S/CB) exhibit improved electrochemical stability as well as enhanced rate performance, evidenced by various electrochemical analyses. The cyclic voltammetry and the galvanostatic cycling analysis revealed that the GO plays key roles in homogenizing the nanocomposite structures of the electrodes, in improving the electrochemical contact, and in minimizing the loss of soluble polysulfide intermediates. An electrochemical impedance spectroscopy analysis also confirms the enhanced structural stability of the GO-S/CB composites after battery operation. As a result, the GO-S/CB exhibited excellent cycle stability and specific capacity as high as ∼723.7 mA h g(-1) even after 100 cycles at 0.5 C.

  2. Analysis of geometric and electrochemical characteristics of lithium cobalt oxide electrode with different packing densities

    DOE PAGES

    Lim, Cheolwoong; Yan, Bo; Kang, Huixiao; ...

    2016-08-06

    In order to investigate geometric and electrochemical characteristics of Li ion battery electrode with different packing densities, lithium cobalt oxide (LiCoO2) cathode electrodes were fabricated from a 94:3:3 (wt%) mixture of LiCoO2, polymeric binder, and super-P carbon black and calendered to different densities. A synchrotron X-ray nano-computed tomography system with a spatial resolution of 58.2 nm at the Advanced Photon Source of the Argonne National Laboratory was employed to obtain three dimensional morphology data of the electrodes. The morphology data were then quantitatively analyzed to characterize their geometric properties, such as porosity, tortuosity, specific surface area, and pore size distribution.more » The geometric and electrochemical analysis reveal that high packing density electrodes have smaller average pore size and narrower pore size distribution, which improves the electrical contact between carbon-binder matrix and LiCoO2 particles. The better contact improves the capacity and rate capability by reducing the possibility of electrically isolated LiCoO2 particles and increasing the electrochemically active area. The results show that increase of packing density results in higher tortuosity, but electrochemically active area is more crucial to cell performance than tortuosity at up to 3.6 g/cm3 packing density and 4 C rate.« less

  3. Analysis of geometric and electrochemical characteristics of lithium cobalt oxide electrode with different packing densities

    SciTech Connect

    Lim, Cheolwoong; Yan, Bo; Kang, Huixiao; Song, Zhibin; Lee, Wen Chao; De Andrade, Vincent; De Carlo, Francesco; Yin, Leilei; Kim, Youngsik; Zhu, Likun

    2016-08-06

    In order to investigate geometric and electrochemical characteristics of Li ion battery electrode with different packing densities, lithium cobalt oxide (LiCoO2) cathode electrodes were fabricated from a 94:3:3 (wt%) mixture of LiCoO2, polymeric binder, and super-P carbon black and calendered to different densities. A synchrotron X-ray nano-computed tomography system with a spatial resolution of 58.2 nm at the Advanced Photon Source of the Argonne National Laboratory was employed to obtain three dimensional morphology data of the electrodes. The morphology data were then quantitatively analyzed to characterize their geometric properties, such as porosity, tortuosity, specific surface area, and pore size distribution. The geometric and electrochemical analysis reveal that high packing density electrodes have smaller average pore size and narrower pore size distribution, which improves the electrical contact between carbon-binder matrix and LiCoO2 particles. The better contact improves the capacity and rate capability by reducing the possibility of electrically isolated LiCoO2 particles and increasing the electrochemically active area. The results show that increase of packing density results in higher tortuosity, but electrochemically active area is more crucial to cell performance than tortuosity at up to 3.6 g/cm3 packing density and 4 C rate.

  4. Analysis of Geometric and Electrochemical Characteristics of Lithium Cobalt Oxide Electrode with Different Packing Densities

    SciTech Connect

    Lim, Cheolwoong; Yan, Bo; Kang, Huixiao; Song, Zhibin; Lee, Wen Chao; De Andrade, Vincent; De Carlo, Francesco; Yin, Leilei; Kim, Youngsik; Zhu, Likun

    2016-10-01

    To investigate geometric and electrochemical characteristics of Li ion battery electrode with different packing densities, lithium cobalt oxide (LiCoO2) cathode electrodes were fabricated from a 94:3:3 (wt%) mixture of LiCoO2, polymeric binder, and super-P carbon black and calendered to different densities. A synchrotron X-ray nano-computed tomography system with a spatial resolution of 58.2 nm at the Advanced Photon Source of the Argonne National Laboratory was employed to obtain three dimensional morphology data of the electrodes. The morphology data were quantitatively analyzed to characterize their geometric properties, such as porosity, tortuosity, specific surface area, and pore size distribution. The geometric and electrochemical analysis reveal that high packing density electrodes have smaller average pore size and narrower pore size distribution, which improves the electrical contact between carbon-binder matrix and LiCoO2 particles. The better contact improves the capacity and rate capability by reducing the possibility of electrically isolated LiCoO2 particles and increasing the electrochemically active area. The results show that increase of packing density results in higher tortuosity, but electrochemically active area is more crucial to cell performance than tortuosity at up to 3.6 g/cm3 packing density and 4 C rate.

  5. Analysis of geometric and electrochemical characteristics of lithium cobalt oxide electrode with different packing densities

    NASA Astrophysics Data System (ADS)

    Lim, Cheolwoong; Yan, Bo; Kang, Huixiao; Song, Zhibin; Lee, Wen Chao; De Andrade, Vincent; De Carlo, Francesco; Yin, Leilei; Kim, Youngsik; Zhu, Likun

    2016-10-01

    To investigate geometric and electrochemical characteristics of Li ion battery electrode with different packing densities, lithium cobalt oxide (LiCoO2) cathode electrodes were fabricated from a 94:3:3 (wt%) mixture of LiCoO2, polymeric binder, and super-P carbon black and calendered to different densities. A synchrotron X-ray nano-computed tomography system with a spatial resolution of 58.2 nm at the Advanced Photon Source of the Argonne National Laboratory was employed to obtain three dimensional morphology data of the electrodes. The morphology data were quantitatively analyzed to characterize their geometric properties, such as porosity, tortuosity, specific surface area, and pore size distribution. The geometric and electrochemical analysis reveal that high packing density electrodes have smaller average pore size and narrower pore size distribution, which improves the electrical contact between carbon-binder matrix and LiCoO2 particles. The better contact improves the capacity and rate capability by reducing the possibility of electrically isolated LiCoO2 particles and increasing the electrochemically active area. The results show that increase of packing density results in higher tortuosity, but electrochemically active area is more crucial to cell performance than tortuosity at up to 3.6 g/cm3 packing density and 4 C rate.

  6. Effect of surfactant on the electrochemical performance of graphene/iron oxide electrode for supercapacitor

    NASA Astrophysics Data System (ADS)

    Ghasemi, Shahram; Ahmadi, Fatemeh

    2015-09-01

    In this study, reduced graphene oxide- Fe3O4 (RGO-Fe3O4) nanocomposite is fabricated using simple electrophoretic deposition (EPD) method followed by an electrochemical reduction process. It is characterized using atomic force microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Raman spectroscopy and scanning electron microscopy. Fe3O4 nanoparticles with 20-50 nm in diameter are uniformly formed on RGO. Electrochemical properties of nanocomposite are characterized by cyclic voltammetery, galvanostatic charge/discharge and electrochemical impedance spectroscopy. According to the galvanostatic charge/discharge analysis, RGO-Fe3O4/SS presents specific capacitance (Cs) of 154 F g-1 at current density of 1 A g-1, which is higher than that of RGO/SS (81 F g-1) in Na2SO4 electrolyte. Also, the electrochemical behaviors show that addition of three kind of surfactant, i.e. sodium dodecyl sulphate, cetyltrimethylammonium bromide, t-octyl phenoxy polyethoxyethanol (Triton X-100) to Na2SO4 aqueous solution can improve the Cs of RGO-Fe3O4/SS electrodes. RGO-Fe3O4/SS in Na2SO4 electrolyte containing Triton X-100 shows maximum Cs of 236 F g-1 at 1 A g-1 which retains 97% of initial capacitance after 500 cycles.

  7. The woven fiber organic electrochemical transistors based on polypyrrole nanowires/reduced graphene oxide composites for glucose sensing.

    PubMed

    Wang, Yuedan; Qing, Xing; Zhou, Quan; Zhang, Yang; Liu, Qiongzhen; Liu, Ke; Wang, Wenwen; Li, Mufang; Lu, Zhentan; Chen, Yuanli; Wang, Dong

    2017-09-15

    Novel woven fiber organic electrochemical transistors based on polypyrrole (PPy) nanowires and reduced graphene oxide (rGO) have been prepared. SEM revealed that the introduction of rGO nanosheets could induce the growth and increase the amount of PPy nanowires. Moreover, it could enhance the electrical performance of fiber transistors. The hybrid transistors showed high on/off ratio of 10(2), fast switch speed, and long cycling stability. The glucose sensors based on the fiber organic electrochemical transistors have also been investigated, which exhibited outstanding sensitivity, as high as 0.773 NCR/decade, with a response time as fast as 0.5s, a linear range of 1nM to 5μM, a low detection concentration as well as good repeatability. In addition, the glucose could be selectively detected in the presence of ascorbic acid and uric acid interferences. The reliability of the proposed glucose sensor was evaluated in real samples of rabbit blood. All the results indicate that the novel fiber transistors pave the way for portable and wearable electronics devices, which have a promising future for healthcare and biological applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. An Elegant Analysis of White Spot Syndrome Virus Using a Graphene Oxide/Methylene Blue based Electrochemical Immunosensor Platform

    NASA Astrophysics Data System (ADS)

    Natarajan, Anusha; Devi, K. S. Shalini; Raja, Sudhakaran; Senthil Kumar, Annamalai

    2017-04-01

    White spot syndrome virus (WSSV) is a major devastating virus in aquaculture industry. A sensitive and selective diagnostic method for WSSV is a pressing need for the early detection and protection of the aquaculture farms. Herein, we first report, a simple electrochemical immunosensor based on methylene blue dye (MB) immobilized graphene oxide modified glassy carbon electrode (GCE/GO@MB) for selective, quick (35 ± 5 mins) and raw sample analysis of WSSV. The immunosensor was prepared by sequential modification of primary antibody, blocking agent (bovine serum album), antigen (as vp28 protein), secondary antibody coupled with horseradish peroxidase (Ab2-HRP) on the GCE/GO@MB. The modified electrode showed a well-defined redox peak at an equilibrium potential (E1/2), -0.4 V vs Ag/AgCl and mediated H2O2 reduction reaction without any false positive result and dissolved oxygen interferences in pH 7 phosphate buffer solution. Under an optimal condition, constructed calibration plot was linear in a range of 1.36 × 10-3 to 1.36 × 107 copies μL-1 of vp28. It is about four orders higher sensitive than that of the values observed with polymerase chain reaction (PCR) and western blot based WSSV detection techniques. Direct electrochemical immunosensing of WSSV in raw tissue samples were successfully demonstrated as a real sample system.

  9. Electrochemical behavior of solid oxide fuel cell anodes based on infiltration of Y-doped SrTiO3

    NASA Astrophysics Data System (ADS)

    Torabi, Alireza; Etsell, Thomas H.

    2013-03-01

    Single cells based on yttrium-doped SrTiO3 (YST) infiltrated porous YSZ anodes were investigated as an alternative material for sulfur and carbon tolerant solid oxide fuel cells. First, a YSZ electrolyte-based cell with porous YSZ as the support for electrode materials on both sides was prepared. Then electrocatalyst materials were incorporated into the porous YSZ: the anode was infiltrated with YST precursor; and the cathode with LSM precursor to be heat treated in-situ. Heat treatment under reducing conditions was found to successfully eliminate the yttrium titanate impurity and to markedly reduce the YST crystal size. The results showed that there was an optimum amount of infiltrated YST to balance the conductivity and the polarization. Furthermore, the maximum power density under dry hydrogen at 900 °C was found to be 95 mW cm-2, which is greater than comparable reported values. H2S was found to have a promoting effect on the electrochemical performance of the fuel cell, particularly under methane. This work suggests that the infiltration technique can be successfully used not only to eliminate the complications associated with high temperature treatments required in conventional YST-YSZ anodes, but also to improve the electrochemical performance.

  10. An Elegant Analysis of White Spot Syndrome Virus Using a Graphene Oxide/Methylene Blue based Electrochemical Immunosensor Platform

    PubMed Central

    Natarajan, Anusha; Devi, K. S. Shalini; Raja, Sudhakaran; Senthil Kumar, Annamalai

    2017-01-01

    White spot syndrome virus (WSSV) is a major devastating virus in aquaculture industry. A sensitive and selective diagnostic method for WSSV is a pressing need for the early detection and protection of the aquaculture farms. Herein, we first report, a simple electrochemical immunosensor based on methylene blue dye (MB) immobilized graphene oxide modified glassy carbon electrode (GCE/GO@MB) for selective, quick (35 ± 5 mins) and raw sample analysis of WSSV. The immunosensor was prepared by sequential modification of primary antibody, blocking agent (bovine serum album), antigen (as vp28 protein), secondary antibody coupled with horseradish peroxidase (Ab2-HRP) on the GCE/GO@MB. The modified electrode showed a well-defined redox peak at an equilibrium potential (E1/2), −0.4 V vs Ag/AgCl and mediated H2O2 reduction reaction without any false positive result and dissolved oxygen interferences in pH 7 phosphate buffer solution. Under an optimal condition, constructed calibration plot was linear in a range of 1.36 × 10−3 to 1.36 × 107 copies μL−1 of vp28. It is about four orders higher sensitive than that of the values observed with polymerase chain reaction (PCR) and western blot based WSSV detection techniques. Direct electrochemical immunosensing of WSSV in raw tissue samples were successfully demonstrated as a real sample system. PMID:28393929

  11. Ag/N-doped reduced graphene oxide incorporated with molecularly imprinted polymer: An advanced electrochemical sensing platform for salbutamol determination.

    PubMed

    Li, Junhua; Xu, Zhifeng; Liu, Mengqin; Deng, Peihong; Tang, Siping; Jiang, Jianbo; Feng, Haibo; Qian, Dong; He, Lingzhi

    2017-04-15

    In this work, the metallic silver and non-metallic nitrogen co-doped reduced graphene oxide (Ag-N-RGO) was first synthesized by a simple and cost-effective strategy, and then a molecularly imprinted polymer (MIP) was formed in situ at the surface of the prepared composite via electropolymerization of o-phenylenediamine in the presence of salbutamol as the template molecule. The electrochemical characterizations demonstrate that the bifunctional graphene-based composite shows improved catalytic performance than that of pristine graphene doped with one-component or none. The MIP sensor based on Ag-N-RGO owns high porous surface structure, resulting in the increased current response and enhanced recognition capacity than that of non-imprinted sensor. The outstanding performance of the developed sensor derives from the combined advantages of Ag-N-RGO with effective catalytic property and MIP with excellent selectivity. Under the optimal conditions, the electrochemical response of the developed sensor is linearly proportional to the concentration of salbutamol in the range of 0.03-20.00µmolL(-1) with a low detection limit of 7 nmol L(-1). The designed sensor has exhibited the multiple advantages such as low cost, simple manufacture, convenient use, excellent selectivity and good reproducibility. Finally, the proposed method has been extended for the determinations of salbutamol in human urine and pork samples, and the satisfactory recoveries between 98.9-105.3% are achieved. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Synthesis and Stabilization of Blue-Black TiO2 Nanotube Arrays for Electrochemical Oxidant Generation and Wastewater Treatment.

    PubMed

    Yang, Yang; Hoffmann, Michael R

    2016-11-01

    Efficient, inexpensive, and stable electrode materials are key components of commercially viable electrochemical wastewater treatment system. In this study, blue-black TiO2 nanotube array (BNTA) electrodes are prepared by electrochemical self-doping. The 1-D structure, donor state density, and Fermi energy level position are critical for maintaining the semimetallic functionality of the BNTA. The structural strength of the BNTA is enhanced by surface crack minimization, reinforcement of the BNTA-Ti metal interface, and stabilized by a protective overcoating with nanoparticulate TiO2 (Ti/EBNTA). Ti/EBNTA electrodes are employed as both anodes and cathodes with polarity switching at a set frequency. Oxidants are generated at the anode, while the doping levels are regenerated along with byproduct reduction at the cathode. The estimated maximum electrode lifetime is 16 895 h. Ti/EBNTA has comparable hydroxyl radical production activity (6.6 × 10(-14) M) with boron-doped diamond (BDD, 7.4 × 10(-14) M) electrodes. The chlorine production rate follows a trend with respective to electrode type of Ti/EBNTA > BDD > IrO2. Ti/EBNTA electrodes operated in a bipolar mode have a minimum energy consumption of 62 kWh/kg COD, reduced foam formation due to less gas bubble production, minimum scale formation, and lower chlorate production levels (6 mM vs 18 mM for BDD) during electrolytic wastewater treatment.

  13. Cerium oxide nanoparticles/multi-wall carbon nanotubes composites: Facile synthesis and electrochemical performances as supercapacitor electrode materials

    NASA Astrophysics Data System (ADS)

    Deng, Dongyang; Chen, Nan; Li, Yuxiu; Xing, Xinxin; Liu, Xu; Xiao, Xuechun; Wang, Yude

    2017-02-01

    Cerium oxide nanoparticles/multi-wall carbon nanotubes (MWCNTs) composites are synthesized by a facile hydrothermal method without any surfactant or template. The morphology and microstructure of samples are examined by scanning electron microscopy (SEM), transition electron microscopy (TEM), X-ray diffraction (XRD), Raman spectrum and X-ray photoelectron spectroscopy (XPS). Electrochemical properties of the MWCNTs, the pure CeO2, and the CeO2/MWCNTs nanocomposites electrodes are investigated by cyclic voltammetry (CV), galvanostatic charge/discharge (GDC) and electrochemical impedance spectroscopy (EIS) measurements. The CeO2/MWCNTs nanocomposite (at the mole ratio of 1:1) electrode exhibits much larger specific capacitance compared with both the MWCNTs electrode and the pure CeO2 electrode and significantly improves cycling stability compared to the pure CeO2 electrode. The CeO2/MWCNTs nanocomposite (at the mole ratio of 1:1) achieves a specific capacitance of 455.6 F g-1 at the current density of 1 A g-1. Therefore, the as prepared CeO2/MWCNTs nanocomposite is a promising electrode material for high-performance supercapacitors.

  14. Preparation and Electrochemical Characterization of a Carbon Ceramic Electrode Modified with Ferrocenecarboxylic Acid

    PubMed Central

    Skeika, Tatiane; Zuconelli, Cristiane R.; Fujiwara, Sergio T.; Pessoa, Christiana A.

    2011-01-01

    The present paper describes the characterization of a carbon ceramic electrode modified with ferrocenecarboxylic acid (designated as CCE/Fc) by electrochemical techniques and its detection ability for dopamine. From cyclic voltammetric experiments, it was observed that the CCE/Fc presented a redox pair at Epa = 405 mV and Epc = 335 mV (ΔE = 70 mV), related to the ferrocene/ferrocenium process. Studies showed a considerably increase in the redox currents at the same oxidation potential of ferrocene (Epa = 414 mV vs. Ag/AgCl) in the presence of dopamine (DA), differently from those observed when using only the unmodified CCE, in which the anodic peak increase was considerably lower. From SWV experiments, it was observed that the AA (ascorbic acid) oxidation at CCE/Fc occurred in a different potential than the DA oxidation (with a peak separation of approximately 200 mV). Moreover, CCE/Fc did not respond to different AA concentrations, indicating that it is possible to determine DA without the AA interference with this electrode. PMID:22319356

  15. Zinc oxide/redox mediator composite films-based sensor for electrochemical detection of important biomolecules.

    PubMed

    Tang, Chun-Fang; Kumar, S Ashok; Chen, Shen-Ming

    2008-09-15

    Electrochemical oxidation of serotonin (SN) onto zinc oxide (ZnO)-coated glassy carbon electrode (GCE) results in the generation of redox mediators (RMs) that are strongly adsorbed on electrode surface. The electrochemical properties of zinc oxide-electrogenerated redox mediator (ZnO/RM) (inorganic/organic) hybrid film-coated electrode has been studied using cyclic voltammetry (CV). The scanning electron microscope (SEM), atomic force microscope (AFM), and electrochemical techniques proved the immobilization of ZnO/RM core/shell microparticles on the electrode surface. The GCE modified with ZnO/RM hybrid film showed two reversible redox peaks in acidic solution, and the redox peaks were found to be pH dependent with slopes of -62 and -60 mV/pH, which are very close to the Nernst behavior. The GCE/ZnO/RM-modified electrode exhibited excellent electrocatalytic activity toward the oxidations of ascorbic acid (AA), dopamine (DA), and uric acid (UA) in 0.1M phosphate buffer solution (PBS, pH 7.0). Indeed, ZnO/RM-coated GCE separated the anodic oxidation waves of DA, AA, and UA with well-defined peak separations in their mixture solution. Consequently, the GCE/ZnO/RMs were used for simultaneous detection of DA, AA, and UA in their mixture solution. Using CV, calibration curves for DA, AA, and UA were obtained over the range of 6.0 x 10(-6) to 9.6 x 10(-4)M, 1.5 x 10(-5) to 2.4 x 10(-4)M, and 5.0 x 10(-5) to 8 x 10(-4)M with correlation coefficients of 0.992, 0.991, and 0.989, respectively. Moreover, ZnO/RM-modified GCE had good stability and antifouling properties.

  16. Molecular Insight in Structure and Activity of Highly Efficient, Low-Ir Ir-Ni Oxide Catalysts for Electrochemical Water Splitting (OER).

    PubMed

    Reier, Tobias; Pawolek, Zarina; Cherevko, Serhiy; Bruns, Michael; Jones, Travis; Teschner, Detre; Selve, Sören; Bergmann, Arno; Nong, Hong Nhan; Schlögl, Robert; Mayrhofer, Karl J J; Strasser, Peter

    2015-10-14

    Mixed bimetallic oxides offer great opportunities for a systematic tuning of electrocatalytic activity and stability. Here, we demonstrate the power of this strategy using well-defined thermally prepared Ir-Ni mixed oxide thin film catalysts for the electrochemical oxygen evolution reaction (OER) under highly corrosive conditions such as in acidic proton exchange membrane (PEM) electrolyzers and photoelectrochemical cells (PEC). Variation of the Ir to Ni ratio resulted in a volcano type OER activity curve with an unprecedented 20-fold improvement in Ir mass-based activity over pure Ir oxide. In situ spectroscopic probing of metal dissolution indicated that, against common views, activity and stability are not directly anticorrelated. To uncover activity and stability controlling parameters, the Ir-Ni mixed thin oxide film catalysts were characterized by a wide array of spectroscopic, microscopic, scattering, and electrochemical techniques in conjunction with DFT theoretical computations. By means of an intuitive model for the formation of the catalytically active state of the bimetallic Ir-Ni oxide surface, we identify the coverage of reactive surface hydroxyl groups as a suitable descriptor for the OER activity and relate it to controllable synthetic parameters. Overall, our study highlights a novel, highly active oxygen evolution catalyst; moreover, it provides novel important insights into the structure and performance of bimetallic oxide OER electrocatalysts in corrosive acidic environments.

  17. Solar-mediated thermo-electrochemical oxidation of sodium dodecyl benzene sulfonate by modulating the effective oxidation potential and pathway for green remediation of wastewater

    PubMed Central

    Gu, Di; Gao, Simeng; Jiang, TingTing; Wang, Baohui

    2017-01-01

    To match the relentless pursuit of three research hot points - efficient solar utilization, green and sustainable remediation of wastewater and advanced oxidation processes, solar-mediated thermo-electrochemical oxidation of surfactant was proposed and developed for green remediation of surfactant wastewater. The solar thermal electrochemical process (STEP), fully driven with solar energy to electric energy and heat and without an input of other energy, sustainably serves as efficient thermo-electrochemical oxidation of surfactant, exemplified by SDBS, in wastewater with the synergistic production of hydrogen. The electrooxidation-resistant surfactant is thermo-electrochemically oxidized to CO2 while hydrogen gas is generated by lowing effective oxidation potential and suppressing the oxidation activation energy originated from the combination of thermochemical and electrochemical effect. A clear conclusion on the mechanism of SDBS degradation can be proposed and discussed based on the theoretical analysis of electrochemical potential by quantum chemical method and experimental analysis of the CV, TG, GC, FT-IR, UV-vis, Fluorescence spectra and TOC. The degradation data provide a pilot for the treatment of SDBS wastewater that appears to occur via desulfonation followed by aromatic-ring opening. The solar thermal utilization that can initiate the desulfonation and activation of SDBS becomes one key step in the degradation process. PMID:28294180

  18. Solar-mediated thermo-electrochemical oxidation of sodium dodecyl benzene sulfonate by modulating the effective oxidation potential and pathway for green remediation of wastewater

    NASA Astrophysics Data System (ADS)

    Gu, Di; Gao, Simeng; Jiang, Tingting; Wang, Baohui

    2017-03-01

    To match the relentless pursuit of three research hot points - efficient solar utilization, green and sustainable remediation of wastewater and advanced oxidation processes, solar-mediated thermo-electrochemical oxidation of surfactant was proposed and developed for green remediation of surfactant wastewater. The solar thermal electrochemical process (STEP), fully driven with solar energy to electric energy and heat and without an input of other energy, sustainably serves as efficient thermo-electrochemical oxidation of surfactant, exemplified by SDBS, in wastewater with the synergistic production of hydrogen. The electrooxidation-resistant surfactant is thermo-electrochemically oxidized to CO2 while hydrogen gas is generated by lowing effective oxidation potential and suppressing the oxidation activation energy originated from the combination of thermochemical and electrochemical effect. A clear conclusion on the mechanism of SDBS degradation can be proposed and discussed based on the theoretical analysis of electrochemical potential by quantum chemical method and experimental analysis of the CV, TG, GC, FT-IR, UV-vis, Fluorescence spectra and TOC. The degradation data provide a pilot for the treatment of SDBS wastewater that appears to occur via desulfonation followed by aromatic-ring opening. The solar thermal utilization that can initiate the desulfonation and activation of SDBS becomes one key step in the degradation process.

  19. Solar-mediated thermo-electrochemical oxidation of sodium dodecyl benzene sulfonate by modulating the effective oxidation potential and pathway for green remediation of wastewater.

    PubMed

    Gu, Di; Gao, Simeng; Jiang, TingTing; Wang, Baohui

    2017-03-15

    To match the relentless pursuit of three research hot points - efficient solar utilization, green and sustainable remediation of wastewater and advanced oxidation processes, solar-mediated thermo-electrochemical oxidation of surfactant was proposed and developed for green remediation of surfactant wastewater. The solar thermal electrochemical process (STEP), fully driven with solar energy to electric energy and heat and without an input of other energy, sustainably serves as efficient thermo-electrochemical oxidation of surfactant, exemplified by SDBS, in wastewater with the synergistic production of hydrogen. The electrooxidation-resistant surfactant is thermo-electrochemically oxidized to CO2 while hydrogen gas is generated by lowing effective oxidation potential and suppressing the oxidation activation energy originated from the combination of thermochemical and electrochemical effect. A clear conclusion on the mechanism of SDBS degradation can be proposed and discussed based on the theoretical analysis of electrochemical potential by quantum chemical method and experimental analysis of the CV, TG, GC, FT-IR, UV-vis, Fluorescence spectra and TOC. The degradation data provide a pilot for the treatment of SDBS wastewater that appears to occur via desulfonation followed by aromatic-ring opening. The solar thermal utilization that can initiate the desulfonation and activation of SDBS becomes one key step in the degradation process.

  20. Synthesis and electrochemical preformances of tribasic and tetrabasic lead sulfates prepared by reactive grinding

    NASA Astrophysics Data System (ADS)

    Grugeon-Dewaele, S.; Laruelle, S.; Joliveau-Vallat, F.; Torcheux, L.; Delahaye-Vidal, A.

    Tribasic lead sulfate (3BS) and tetrabasic lead sulfate (4BS), used as precursors of the positive active material in the lead/acid batteries, were prepared by a new method: reactive grinding. The effects of various experimental parameters (stoichiometry, hygrometry of the starting compounds, duration of mechanical treatment) upon the nature and morphological features of the resulting phase were investigated. Among them, hygrometry turned out to be the most critical one. With water in excess, only 3BS was produced while dry reagents led to 4BS. In both cases, samples with a small particle size and high reactivity were obtained. In order to evaluate the influence of the morphology upon the electrochemical performances of such grinding produced samples, the capacity was measured and compared with that of traditional 3BS and 4BS samples.

  1. Preparation of electrochemical sensor for lead(II) based on molecularly imprinted film

    NASA Astrophysics Data System (ADS)

    Wang, Zhihua; Qin, Yaxin; Wang, Chu; Sun, Lijun; Lu, Xiaole; Lu, Xiaoquan

    2012-01-01

    A high selective voltammetric sensor for Pb2+ was introduced. The feasibility of utilizing strong interactions between Schiff bases and metal ion to prepare the molecularly imprinted polymers (MIPs) electrochemical sensor for Pb2+ in aqueous solutions was studied. Some parameters affecting sensor response were optimized and then a calibration curve was plotted. A dynamic linear range of 3.00 × 10-7 to 5.00 × 10-5 mol/L was obtained. The redox process of Pb2+ on the imprinted electrode is controlled by surface reaction. The stability and the life of imprinted membrane were improved by storing into diluted Pb2+ ion solution. The proposed method was applied to determination of Pb2+ in the Yellow River.

  2. Charge Transport Properties of P3HT-PEO block copolymers that are Electrochemically Oxidized in the Solid-State

    NASA Astrophysics Data System (ADS)

    Patel, Shrayesh; Javier, Anna; Balsara, Nitash

    2013-03-01

    We report on the relationship between morphology and electronic/ionic charge transport of Poly(3-hexylthiophene)- b-Poly(ethylene oxide) (P3HT- b-PEO) and lithium bis-(trifluoromethanesulfonyl) imide (LiTFSI) mixtures. Using ac impedance spectroscopy, we show that P3HT- b-PEO/LiTFSI mixtures can conduct electronic and ionic charges simultaneously. The electronic resistance of P3HT- b-PEO can be controlled through the electrochemical oxidation of P3HT with LiTFSI. We designed an all solid-state electrochemical cell with three terminals to measure the electronic conductivity of P3HT- b-PEO under applied potentials. The addition of a third terminal within the P3HT- b-PEO layer allows for the in-situ measurement of the electronic conductivity as a function of the P3HT electrochemical oxidation level. Our experimental setup is unique in that electrochemical oxidation occurs in the presence of solid-polymer electrolyte. Previous studies on the electrochemical oxidation of polythiophenes have been done in the presence of a liquid electrolyte. The results of the in-situ electronic conductivity measurements as a function of electrochemical doping level and block copolymer composition will be presented.

  3. Electrochemical properties of tungsten sulfide–carbon composite microspheres prepared by spray pyrolysis

    PubMed Central

    Choi, Seung Ho; Boo, Sung Jin; Lee, Jong-Heun; Kang, Yun Chan

    2014-01-01

    Tungsten sulfide (WS2)–carbon composite powders with superior electrochemical properties are prepared by a two-step process. WO3-carbon composite powders were first prepared by conventional spray pyrolysis, and they were then sulfidated to form WS2-carbon powders. Bare WS2 powders are also prepared by sulfidation of bare WO3 powders obtained by spray pyrolysis. Stacked graphitic layers could not be found in the bare WS2 and WS2–carbon composite powders. The amorphous bare WS2 and WS2–carbon composite powders have Brunauer–Emmett–Teller (BET) surface areas of 2.8 and 4 m2 g−1, respectively. The initial discharge and charge capacities of the WS2–carbon composite powders at a current density of 100 mA g−1 are 1055 and 714 mA h g−1, respectively, and the corresponding initial Coulombic efficiency is 68%. On the other hand, the initial discharge and charge capacities of the bare WS2 powders are 514 and 346 mA h g−1, respectively. The discharge capacities of the WS2–carbon composite powders for the 2nd and 50th cycles are 716 and 555 mA h g−1, respectively, and the corresponding capacity retention measured after first cycle is 78%. PMID:25169439

  4. Electrochemical preparation of Photosystem I-polyaniline composite films for biohybrid solar energy conversion.

    PubMed

    Gizzie, Evan A; LeBlanc, Gabriel; Jennings, G Kane; Cliffel, David E

    2015-05-13

    In this work, we report for the first time the entrapment of the biomolecular supercomplex Photosystem I (PSI) within a conductive polymer network of polyaniline via electrochemical copolymerization. Composite polymer-protein films were prepared on gold electrodes through potentiostatic electropolymerization from a single aqueous solution containing both aniline and PSI. This study demonstrates the controllable integration of large membrane proteins into rapidly prepared composite films, the entrapment of such proteins was observed through photoelectrochemical analysis. PSI's unique function as a highly efficient biomolecular photodiode generated a significant enhancement in photocurrent generation for the PSI-loaded polyaniline films, compared to pristine polyaniline films, and dropcast PSI films. A comprehensive study was then performed to separately evaluate film thickness and PSI concentration in the initial polymerization solution and their effects on the net photocurrent of this novel material. The best performing composite films were prepared with 0.1 μM PSI in the polymerization solution and deposited to a film thickness of 185 nm, resulting in an average photocurrent density of 5.7 μA cm(-2) with an efficiency of 0.005%. This photocurrent output represents an enhancement greater than 2-fold over bare polyaniline films and 200-fold over a traditional PSI multilayer film of comparable thickness.

  5. A novel ultrafine leady oxide prepared from spent lead pastes for application as cathode of lead acid battery

    NASA Astrophysics Data System (ADS)

    Yang, Danni; Liu, Jianwen; Wang, Qin; Yuan, Xiqing; Zhu, Xinfeng; Li, Lei; Zhang, Wei; Hu, Yuchen; Sun, Xiaojuan; Kumar, R. Vasant; Yang, Jiakuan

    2014-07-01

    A novel ultrafine leady oxide has been prepared from a combustion-calcination process of lead citrate precursor (Pb3(C6H5O7)2·3H2O), by hydrometallurgical leaching of spent lead pastes firstly. The leady oxides are used to assemble lead acid battery which are subjected to cyclic voltammetry (CV) and battery testing. Various key properties of the new oxides, such as morphology, crystalline phases, degree of oxidation, apparent density and water and acid absorption value have been characterized by chemical analysis, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results show that leady oxides synthesized at different calcination temperatures mainly comprise β-PbO, α-PbO and Pb. Unlike traditional leady oxide, the new oxide product prepared at 375 °C has a rod-like morphology with greater porous structure, and appears smaller density, lower value of acid absorption and larger propensity for water absorption. In battery testing, the 20 h rate and 1C rate discharge time have exceeded 26 h and 40 min, respectively. Results reveal that the leady oxide prepared at 375 °C exhibits excellent electrochemical performance and initial capacity as positive active material. While leady oxide obtained at 450 °C presents a relatively improved cycle life. Further work is to optimize the battery manufacturing process for better cycle performance.

  6. Efficient electrochemical oxidation of perfluorooctanoate using a Ti/SnO2-Sb-Bi anode.

    PubMed

    Zhuo, Qiongfang; Deng, Shubo; Yang, Bo; Huang, Jun; Yu, Gang

    2011-04-01

    The electrochemical decomposition of persistent perfluorooctanoate (PFOA) with a Ti/SnO2-Sb-Bi electrode was demonstrated in this study. After 2 h electrolysis, over 99% of PFOA (25 mL of 50 mg·L(-1)) was degraded with a first-order kinetic constant of 1.93 h(-1). The intermediate products including short-chain perfluorocarboxyl anions (CF3COO-, C2F5COO-, C3F7COO-, C4F9COO-, C5F11COO-, and C6F13COO-) and F- were detected in the aqueous solution. The electrochemical oxidation mechanism was revealed, that PFOA decomposition first occurred through a direct one electron transfer from the carboxyl group in PFOA to the anode at the potential of 3.37 V (vs saturated calomel electrode, SCE). After that, the PFOA radical was decarboxylated to form perfluoroheptyl radical which allowed a defluorination reaction between perfluoroheptyl radical and hydroxyl radical/O2. Electrospray ionization (ESI) mass spectrum further confirmed that the oxidation of PFOA on the Ti/SnO2-Sb-Bi electrode proceeded from the carboxyl group in PFOA rather than C-C cleavage, and the decomposition processes followed the CF2 unzipping cycle. The electrochemical technique with the Ti/SnO2-Sb-Bi electrode provided a potential method for PFOA degradation in the aqueous solution.

  7. Boron doped ZnO embedded into reduced graphene oxide for electrochemical supercapacitors

    NASA Astrophysics Data System (ADS)

    Alver, Ü.; Tanrıverdi, A.

    2016-08-01

    In this work, reduced graphene oxide/boron doped zinc oxide (RGO/ZnO:B) composites were fabricated by a hydrothermal process and their electrochemical properties were investigated as a function of dopant concentration. First, boron doped ZnO (ZnO:B) particles was fabricated with different boron concentrations (5, 10, 15 and 20 wt%) and then ZnO:B particles were embedded into RGO sheets. The physical properties of sensitized composites were characterized by XRD and SEM. Characterization indicated that the ZnO:B particles with plate-like structure in the composite were dispersed on graphene sheets. The electrochemical properties of the RGO/ZnO:B composite were investigated through cyclic voltammetry, galvanostatic charge/discharge measurements in a 6 M KOH electrolyte. Electrochemical measurements show that the specific capacitance values of RGO/ZnO:B electrodes increase with increasing boron concentration. RGO/ZnO:B composite electrodes (20 wt% B) display the specific capacitance as high as 230.50 F/g at 5 mV/s, which is almost five times higher than that of RGO/ZnO (52.71 F/g).

  8. Electrochemical oxidation of biological pretreated and membrane separated landfill leachate concentrates on boron doped diamond anode

    NASA Astrophysics Data System (ADS)

    Zhou, Bo; Yu, Zhiming; Wei, Qiuping; Long, HangYu; Xie, Youneng; Wang, Yijia

    2016-07-01

    In the present study, the high quality boron-doped diamond (BDD) electrodes with excellent electrochemical properties were deposited on niobium (Nb) substrates by hot filament chemical vapor deposition (HFCVD) method. The electrochemical oxidation of landfill leachate concentrates from disc tube reverse osmosis (DTRO) process over a BDD anode was investigated. The effects of varying operating parameters, such as current density, initial pH, flow velocity and cathode material on degradation efficiency were also evaluated following changes in chemical oxygen demand (COD) and ammonium nitrogen (NH3sbnd N). The instantaneous current efficiency (ICE) was used to appraise different operating conditions. As a result, the best conditions obtained were as follows, current density 50 mA cm-2, pH 5.16, flow velocity 6 L h-1. Under these conditions, 87.5% COD and 74.06% NH3sbnd N removal were achieved after 6 h treatment, with specific energy consumption of 223.2 kWh m-3. In short, these results indicated that the electrochemical oxidation with BDD/Nb anode is an effective method for the treatment of landfill leachate concentrates.

  9. Bio-functionalized graphene-graphene oxide nanocomposite based electrochemical immunosensing.

    PubMed

    Sharma, Priyanka; Tuteja, Satish K; Bhalla, Vijayender; Shekhawat, G; Dravid, Vinayak P; Suri, C Raman

    2013-01-15

    We report a novel in-situ electrochemical synthesis approach for the formation of functionalized graphene-graphene oxide (fG-GO) nanocomposite on screen-printed electrodes (SPE). Electrochemically controlled nanocomposite film formation was studied by transmission electron microscopy (TEM) and Raman spectroscopy. Further insight into the nanocomposite has been accomplished by the Fourier transformed infrared spectroscopy (FTIR), thermal gravimetric analysis (TGA) and X-ray diffraction (XRD) spectroscopy. Configured as a highly responsive screen-printed immunosensor, the fG-GO nanocomposite on SPE exhibits electrical and chemical synergies of the nano-hybrid functional construct by combining good electronic properties of functionalized graphene (fG) and the facile chemical functionality of graphene oxide (GO) for compatible bio-interface development using specific anti-diuron antibody. The enhanced electrical properties of nanocomposite biofilm demonstrated a significant increase in electrochemical signal response in a competitive inhibition immunoassay format for diuron detection, promising its potential applicability for ultra-sensitive detection of range of target analytes. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Electrochemical regeneration of Fe2+ in Fenton oxidation processes.

    PubMed

    Qiang, Zhimin; Chang, Jih-Hsing; Huang, Chin-Pao

    2003-03-01

    This study is to establish optimal conditions for the minimization of iron sludge produced in Fenton oxidation processes by electro-regenerating Fe(2+) with constant potential (CPM) or constant current mode (CCM). Results indicate that the optimal cathodic potential for Fe(2+) regeneration is -0.1 V vs. the saturated calomel electrode (SCE) in terms of current efficiency. Keeping the initial Fe(3+) concentration ([Fe(3+)](0)) constant, the average current density produced at -0.1 V vs. SCE (CPM) is approximately equal to the optimal current density applied in the CCM. The suitable pH range is below the pH value determined by Fe(3+) hydrolysis. As expected, increasing cathode surface area and solution temperature notably increases Fe(2+) regeneration rate. At the optimal potential, the average current density increases linearly with [Fe(3+)](0), exhibiting a slope of 8.48 x 10(-3)(A/m(2))(mg/L)(-1). The average current efficiency varies with [Fe(3+)](0), e.g., 75% and 96-98% at 100 and > or = 500 mg/L [Fe(3+)](0), respectively. Once reaching 75% of Fe(2+) regeneration capacity, further regeneration becomes difficult due to Fe(3+) mass transfer limitation. Fe(2+) can also be effectively regenerated by dissolving iron sludge at low pH (usually

  11. Preparation and electrochemical performances of carbon sphere@ZnO core-shell nanocomposites for supercapacitor applications

    PubMed Central

    Xiao, Xuechun; Han, Bingqian; Chen, Gang; Wang, Lihong; Wang, Yude

    2017-01-01

    Carbon sphere (CS)@ZnO core-shell nanocomposites were successfully prepared through facile low-temperature water-bath method without annealing treatment. The morphology and the microstructure of samples were characterized by transition electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), respectively. ZnO nanoparticles with several nanometers in size decorated on the surface of the carbon sphere and formed a core-shell structure. Electrochemical performances of the CS@ZnO core-shell nanocomposites electrodes were investigated by cyclic voltammetry (CV) and galvanostatic charge/discharge (GDC). The CS@ZnO core-shell nanocomposite electrodes exhibit much larger specific capacitance and cycling stability is improved significantly compared with pure ZnO electrode. The CS@ZnO core-shell nanocomposite with mole ratio of 1:1 achieves a specific capacitance of 630 F g−1 at the current density of 2 A g−1. Present work might provide a new route for fabricating carbon sphere and transition metal oxides composite materials as electrodes for the application in supercapacitors. PMID:28057915

  12. Preparation and electrochemical performances of carbon sphere@ZnO core-shell nanocomposites for supercapacitor applications

    NASA Astrophysics Data System (ADS)

    Xiao, Xuechun; Han, Bingqian; Chen, Gang; Wang, Lihong; Wang, Yude

    2017-01-01

    Carbon sphere (CS)@ZnO core-shell nanocomposites were successfully prepared through facile low-temperature water-bath method without annealing treatment. The morphology and the microstructure of samples were characterized by transition electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), respectively. ZnO nanoparticles with several nanometers in size decorated on the surface of the carbon sphere and formed a core-shell structure. Electrochemical performances of the CS@ZnO core-shell nanocomposites electrodes were investigated by cyclic voltammetry (CV) and galvanostatic charge/discharge (GDC). The CS@ZnO core-shell nanocomposite electrodes exhibit much larger specific capacitance and cycling stability is improved significantly compared with pure ZnO electrode. The CS@ZnO core-shell nanocomposite with mole ratio of 1:1 achieves a specific capacitance of 630 F g-1 at the current density of 2 A g-1. Present work might provide a new route for fabricating carbon sphere and transition metal oxides composite materials as electrodes for the application in supercapacitors.

  13. Lithium intercalation in sputter deposited antimony-doped tin oxide thin films: Evidence from electrochemical and optical measurements

    SciTech Connect

    Montero, J. Granqvist, C. G.; Niklasson, G. A.; Guillén, C.; Herrero, J.

    2014-04-21

    Transparent conducting oxides are used as transparent electrical contacts in a variety of applications, including in electrochromic smart windows. In the present work, we performed a study of transparent conducting antimony-doped tin oxide (ATO) thin films by chronopotentiometry in a Li{sup +}-containing electrolyte. The open circuit potential vs. Li was used to investigate ATO band lineups, such as those of the Fermi level and the ionization potential, as well as the dependence of these lineups on the preparation conditions for ATO. Evidence was found for Li{sup +} intercalation when a current pulse was set in a way so as to drive ions from the electrolyte into the ATO lattice. Galvanostatic intermittent titration was then applied to determine the lithium diffusion coefficient within the ATO lattice. The electrochemical density of states of the conducting oxide was studied by means of the transient voltage recorded during the chronopotentiometry experiments. These measurements were possible because, as Li{sup +} intercalation took place, charge compensating electrons filled the lowest part of the conduction band in ATO. Furthermore, the charge insertion modified the optical properties of ATO according to the Drude model.

  14. Lithium intercalation in sputter deposited antimony-doped tin oxide thin films: Evidence from electrochemical and optical measurements

    NASA Astrophysics Data System (ADS)

    Montero, J.; Guillén, C.; Granqvist, C. G.; Herrero, J.; Niklasson, G. A.

    2014-04-01

    Transparent conducting oxides are used as transparent electrical contacts in a variety of applications, including in electrochromic smart windows. In the present work, we performed a study of transparent conducting antimony-doped tin oxide (ATO) thin films by chronopotentiometry in a Li+-containing electrolyte. The open circuit potential vs. Li was used to investigate ATO band lineups, such as those of the Fermi level and the ionization potential, as well as the dependence of these lineups on the preparation conditions for ATO. Evidence was found for Li+ intercalation when a current pulse was set in a way so as to drive ions from the electrolyte into the ATO lattice. Galvanostatic intermittent titration was then applied to determine the lithium diffusion coefficient within the ATO lattice. The electrochemical density of states of the conducting oxide was studied by means of the transient voltage recorded during the chronopotentiometry experiments. These measurements were possible because, as Li+ intercalation took place, charge compensating electrons filled the lowest part of the conduction band in ATO. Furthermore, the charge insertion modified the optical properties of ATO according to the Drude model.

  15. Flexible n-Type High-Performance Thermoelectric Thin Films of Poly(nickel-ethylenetetrathiolate) Prepared by an Electrochemical Method.

    PubMed

    Sun, Yuanhui; Qiu, Lin; Tang, Liangpo; Geng, Hua; Wang, Hanfu; Zhang, Fengjiao; Huang, Dazhen; Xu, Wei; Yue, Peng; Guan, Ying-Shi; Jiao, Fei; Sun, Yimeng; Tang, Dawei; Di, Chong-An; Yi, Yuanping; Zhu, Daoben

    2016-05-01

    Flexible thin films of poly(nickel-ethylenetetrathiolate) prepared by an electrochemical method display promising n-type thermoelectric properties with the highest ZT value up to 0.3 at room temperature. Coexistence of high electrical conductivity and high Seebeck coefficient in this coordination polymer is attributed to its degenerate narrow-bandgap semiconductor behavior.

  16. A novel method for photodegradation of high-chroma dye wastewater via electrochemical pre-oxidation.

    PubMed

    Zhao, Kunjiao; Zhao, Guohua; Li, Peiqiang; Gao, Junxia; Lv, Baoying; Li, Dongming

    2010-06-01

    A new two-step process involving the electrocatalytic (EC) pre-oxidation and the following photoelectrocatalytic synergistic (PEC) oxidation is proposed to treat the high concentration and high-chroma methyl orange dye wastewater, which cannot be degraded by photocatalytic oxidation (PC) directly. The SnO(2)/TiO(2)-NTs/Ti electrode simultaneously possessing the outstanding PC oxidation properties of TiO(2)-NTs and the excellent EC oxidation abilities of the Sb doped SnO(2) was synthesized by impregnating Sb doped SnO(2) nanoparticles into TiO(2)-NTs. In the pre-oxidation process as the first stage, the high-color dye wastewater is decolorized with electrochemical method to some extent. Then, the wastewater becomes a light transmission system. It provides a suitable condition for PC oxidation reaction in the second stage. The synergistic effects of PC and EC oxidation led to the high PEC efficiency and the complete mineralization of dye wastewater is achieved. This two-step process is fast and efficient, which is worthy to study and explore in the practical environmental treatment.

  17. Nanoporous gold supported cobalt oxide microelectrodes as high-performance electrochemical biosensors.

    PubMed

    Lang, Xing-You; Fu, Hong-Ying; Hou, Chao; Han, Gao-Feng; Yang, Ping; Liu, Yong-Bing; Jiang, Qing

    2013-01-01

    Tremendous demands for electrochemical biosensors with high sensitivity and reliability, fast response and excellent selectivity have stimulated intensive research on developing versatile materials with ultrahigh electrocatalytic activity. Here we report flexible and self-supported microelectrodes with a seamless solid/nanoporous gold/cobalt oxide hybrid structure for electrochemical nonenzymatic glucose biosensors. As a result of synergistic electrocatalytic activity of the gold skeleton and cobalt oxide nanoparticles towards glucose oxidation, amperometric glucose biosensors based on the hybrid microelectrodes exhibit multi-linear detection ranges with ultrahigh sensitivities at a low potential of 0.26 V (versus Ag/AgCl). The sensitivity up to 12.5 mA mM⁻¹ cm⁻² with a short response time of less than 1 s gives rise to ultralow detection limit of 5 nM. The outstanding performance originates from a novel nanoarchitecture in which the cobalt oxide nanoparticles are incorporated into pore channels of the seamless solid/nanoporous Au microwires, providing excellent electronic/ionic conductivity and mass transport for the enhanced electrocatalysis.

  18. Electrochemical Water Oxidation by a Catalyst-Modified Metal-Organic Framework Thin Film

    SciTech Connect

    Lin, Shaoyang; Pineda-Galvan, Yuliana; Maza, William A.; Epley, Charity C.; Zhu, Jie; Kessinger, Matthew C.; Pushkar, Yulia; Morris, Amanda J.

    2016-12-15

    Water oxidation, a key component in artificial photosynthesis, requires high overpotentials and exhibits slow reaction kinetics that necessitates the use of stable and efficient heterogeneous water-oxidation catalysts (WOCs). Here, we report the synthesis of UiO-67 metal–organic framework (MOF) thin films doped with [Ru(tpy)(dcbpy)OH2]2+ (tpy=2,2':6',2''-terpyridine, dcbpy=5,5'-dicarboxy-2,2'-bipyridine) on conducting surfaces and their propensity for electrochemical water oxidation. The electrocatalyst oxidized water with a turnover frequency (TOF) of (0.2±0.1) s-1 at 1.71 V versus the normal hydrogen electrode (NHE) in buffered solution (pH~7) and exhibited structural and electrochemical stability. The electroactive sites were distributed throughout the MOF thin film on the basis of scan-ratedependent voltammetry studies. This work demonstrates a promising way to immobilize large concentrations of electroactive WOCs into a highly robust MOF scaffold and paves the way for future photoelectrochemical water-splitting systems.

  19. Optimization and electrochemical characterization of RF-sputtered iridium oxide microelectrodes for electrical stimulation

    NASA Astrophysics Data System (ADS)

    Kang, Xiaoyang; Liu, Jingquan; Tian, Hongchang; Yang, Bin; NuLi, Yanna; Yang, Chunsheng

    2014-02-01

    A reactively sputtered iridium oxide (IrOx) thin film has been developed as electrochemical modification material for microelectrodes to obtain high stability and charge storage capacity (CSC) in functional electrical stimulation. The effect of the oxygen flow and oxygen to argon ratio during sputtering process on the microstructure and electrochemical properties of the IrOx film is characterized. After optimization, the activated IrOx microelectrode shows the highest CSC of 36.15 mC cm-2 at oxygen flow of 25 sccm and oxygen to argon ratio of (2.5:1). Because the deposition process of the reactively sputtered iridium oxide is an exothermic reaction, it is difficult to form film patterning by the lift-off process. The lift-off process was focused on the partially carbonized photoresist (PR) and normal PR. The higher of the carbonization degree of PR reaches, the longer the immersion duration. However, the patterning process of the iridium oxide film becomes feasible when the sputtering pressure is increasing. The experimental results show that the iridium oxide films forms the pattern with the lowest duration of ultrasonic agitation when the deposition pressure is 4.2 Pa and pressure ratio between O2 and Ar pressure is 3:4.

  20. Self-Powered Electrochemical Oxidation of 4-Aminoazobenzene Driven by a Triboelectric Nanogenerator.

    PubMed

    Gao, Shuyan; Su, Jingzhen; Wei, Xianjun; Wang, Miao; Tian, Miao; Jiang, Tao; Wang, Zhong Lin

    2017-01-24

    A rotary disc-structured triboelectric nanogenerator (rd-TENG) on the basis of free-standing electrification has been designed, where the aluminum composite panel has not been tailored to the stator becauseit is commercially available and cost-effective, has good electronic conductivity, and is easily processed. With the rotating speed increasing from 200 to 1000 rpm, the short-circuit current (Isc) is sharply enhanced from 50 μA to 200 μA, while the measured open-circuit voltage (Voc) and transferred charge (Qtr) almost keep constant, 600 V and 0.4 μC, respectively. The matched load for the rd-TENG at a rotating speed of 600 rpm is 2.7 MΩ, generating a maximum power of 19.75 mW, which corresponds to a maximum power density of 2.28 W m(-2). Using the electric power generated by such a rd-TENG, highly toxic and carcinogenic 4-aminoazobenzene can be selectively treated to produce CO2 or an oligomer via reasonably controlling electrochemical oxidation potentials. The underlying mechanism is tentatively proposed based on the cyclic voltammogram, gas chromatograph-mass spectrometer, electrochemical impedance spectroscopy, and UV-vis spectra. Here the electrochemical degradation in a single-compartment cell is more valid, preferable, and feasible. The output Voc and rectified current of rd-TENG guarantee its extensive application to self-power electrochemical degradation of other azo compounds, i.e., 2-(4-dimethylaminophenylazo) benzoic acid, to CO2. This work suggests that rd-TENG, sustainable energy, can be feasibly designed to self-power a practical electrochemical treatment of dyeing wastewater by harvesting vibration energy.