Science.gov

Sample records for potentiostats

  1. Potentiostatic study of a lead dioxide electrode

    SciTech Connect

    Aguf, I.A.; Rasina, O.Z.

    1986-01-01

    The results of a potentiostatic study of a porous lead dioxide electrode indicate that the degree of oxidation of the lead dioxide increases with an increase in the anodic potential, approaching some limit value. A decrease in the anodic potential results in cathodic reduction of some of the oxygen from the crystal lattice of the oxide. Use of the data from the electrostatic and potentiostatic study of the electrode permits calculating the dependence of the oxygen activity in the lead dioxide phase on the anodic potential and degree of oxidation of the oxide.

  2. Wide Dynamic Range CMOS Potentiostat for Amperometric Chemical Sensor

    PubMed Central

    Wang, Wei-Song; Kuo, Wei-Ting; Huang, Hong-Yi; Luo, Ching-Hsing

    2010-01-01

    Presented is a single-ended potentiostat topology with a new interface connection between sensor electrodes and potentiostat circuit to avoid deviation of cell voltage and linearly convert the cell current into voltage signal. Additionally, due to the increased harmonic distortion quantity when detecting low-level sensor current, the performance of potentiostat linearity which causes the detectable current and dynamic range to be limited is relatively decreased. Thus, to alleviate these irregularities, a fully-differential potentiostat is designed with a wide output voltage swing compared to single-ended potentiostat. Two proposed potentiostats were implemented using TSMC 0.18-μm CMOS process for biomedical application. Measurement results show that the fully differential potentiostat performs relatively better in terms of linearity when measuring current from 500 pA to 10 uA. Besides, the dynamic range value can reach a value of 86 dB. PMID:22294899

  3. Instrumentation for potentiostatic corrosion studies with distilled water

    NASA Technical Reports Server (NTRS)

    Loess, R. E.; Youngdahl, C. A.

    1969-01-01

    Corrosion is studied potentiostatically in the corroding environment of distilled water with an instrument that measures the potential of the corroding specimen immediately after interruption of the polarizing current. No current is flowing. The process permits compensation for IR drops when potentiostatic control is used in high resistance systems.

  4. A wireless potentiostat for mobile chemical sensing and biosensing.

    PubMed

    Steinberg, Matthew D; Kassal, Petar; Kereković, Irena; Steinberg, Ivana Murković

    2015-10-01

    Wireless chemical sensors are used as analytical devices in homeland defence, home-based healthcare, food logistics and more generally for the Sensor Internet of Things (SIoT). Presented here is a battery-powered and highly portable credit-card size potentiostat that is suitable for performing mobile and wearable amperometric electrochemical measurements with seamless wireless data transfer to mobile computing devices. The mobile electrochemical analytical system has been evaluated in the laboratory with a model redox system - the reduction of hexacyanoferrate(III) - and also with commercially available enzymatic blood-glucose test-strips. The potentiostat communicates wirelessly with mobile devices such as tablets or Smartphones by near-field communication (NFC) or with personal computers by radio-frequency identification (RFID), and thus provides a solution to the 'missing link' in connectivity that often exists between low-cost mobile and wearable chemical sensors and ubiquitous mobile computing products. The mobile potentiostat has been evaluated in the laboratory with a set of proof-of-concept experiments, and its analytical performance compared with a commercial laboratory potentiostat (R(2)=0.9999). These first experimental results demonstrate the functionality of the wireless potentiostat and suggest that the device could be suitable for wearable and point-of-sample analytical measurements. We conclude that the wireless potentiostat could contribute significantly to the advancement of mobile chemical sensor research and adoption, in particular for wearable sensors in healthcare and sport physiology, for wound monitoring and in mobile point-of-sample diagnostics as well as more generally as a part of the Sensor Internet of Things. PMID:26078146

  5. Development of a low cost potentiostat using ATXMEGA32

    NASA Astrophysics Data System (ADS)

    Muid, Abdul; Djamal, Mitra; Wirawan, Rahadi

    2014-03-01

    Potentiostat is principal devices in modern electrochemical research especially in the investigation of mechanism reaction which associated with the redox chemistry reaction and other chemical phenomena. Several applications measurement is developed based on this tool such as measurement of sample concentrations, quality test of food and medicine, environmental monitoring and biosensors or development of a protein sensor. We have developed a low cost, simple and portable potentiostat with a relatively small dimension. TLC2264 op-amp and ATMEGA32 microcontroller is used to build controller circuit system. Range potential measurement of this tool is between -1600mV and +1600mV within frequency range 1Hz - 1 kHz. The developed instrument has been tested for measuring samples using different voltammetry techniques, like cyclic, square wave, and linear sweep with relative error under 2.5%.

  6. Localized corrosion of container materials under potentiodynamic and potentiostatic controls

    SciTech Connect

    Roy, A.K.; Fleming, D.L.; Gordon, S.R.

    1996-05-01

    Potentiodynamic and potentiostatic polarization experiments were performed on ten candidate waste package container materials to evaluate their pitting tendency at ambient and elevated temperatures in aqueous environments relevant to the potential underground nuclear waste repository. Results indicate that of all the materials tested, Alloys G-30, C-4 and C-22, and Ti Gr-12 exhibited the maximum corrosion resistance, showing no pitting or observable dissolution in any environment tested. These experimental results will be used in identifying a group of potential container materials having the desired corrosion resistance.

  7. Potentiostatic current and galvanostatic potential oscillations during electrodeposition of cadmium.

    PubMed

    López-Sauri, D A; Veleva, L; Pérez-Ángel, G

    2015-09-14

    Cathodic current and potential oscillations were observed during electrodeposition of cadmium from a cyanide electrolyte on a vertical platinum electrode, in potentiostatic and galvanostatic experiments. Electrochemical impedance spectroscopy experiments revealed a region of negative real impedance in a range of non-zero frequencies, in the second descending branch with a positive slope of the N-shape current-potential curve. This kind of dynamical behaviour is characteristic of the HN-NDR oscillators (oscillators with the N-Shape current-potential curve and hidden negative differential resistance). The oscillations could be mainly attributed to the changes in the real active cathodic area, due to the adsorption of hydrogen molecules and their detachment from the surface. The instabilities of the electrochemical processes were characterized by time series, Fast Fourier Transforms and 2-D phase portraits showing quasi-periodic oscillations. PMID:26243301

  8. Metastable pitting of carbon steel under potentiostatic control

    SciTech Connect

    Cheng, Y.F.; Luo, J.L.

    1999-03-01

    The metastable pitting of A516-70 carbon steel was studied under potentiostatic control in solutions containing chloride ions. It was shown that there were different current fluctuation patterns and spectral slopes, that is, roll-off slopes, in passivity, general corrosion, and metastable pitting. Pits were often covered by a deposit which played an important role in the current fluctuation, with a quick current rise followed by a slow drop. There was a transitional potential (about 0 mV vs Ag/AgCl electrode) below which the metastable pitting initiation rate increased with the potential, because more sites would be activated. Above the transitional potential, the decay of the pitting occurrence rate with increased potential was due to the elimination of available pit sites. When the applied potential was between {minus}50 and 100 mV, pit growth kinetics was controlled by the potential drop through the deposit over the pit mouth. The potential dependence of repassivation time was mainly due to the effect of applied potential on the deposit over the pit mouth. There seemed to be good agreement between the calculated pit size and the measured values by optical microphotography. The assumption of hemispherical pit geometry was reasonable in calculating the pit radii.

  9. DStat: A Versatile, Open-Source Potentiostat for Electroanalysis and Integration

    PubMed Central

    Dryden, Michael D. M.; Wheeler, Aaron R.

    2015-01-01

    Most electroanalytical techniques require the precise control of the potentials in an electrochemical cell using a potentiostat. Commercial potentiostats function as “black boxes,” giving limited information about their circuitry and behaviour which can make development of new measurement techniques and integration with other instruments challenging. Recently, a number of lab-built potentiostats have emerged with various design goals including low manufacturing cost and field-portability, but notably lacking is an accessible potentiostat designed for general lab use, focusing on measurement quality combined with ease of use and versatility. To fill this gap, we introduce DStat (http://microfluidics.utoronto.ca/dstat), an open-source, general-purpose potentiostat for use alone or integrated with other instruments. DStat offers picoampere current measurement capabilities, a compact USB-powered design, and user-friendly cross-platform software. DStat is easy and inexpensive to build, may be modified freely, and achieves good performance at low current levels not accessible to other lab-built instruments. In head-to-head tests, DStat’s voltammetric measurements are much more sensitive than those of “CheapStat” (a popular open-source potentiostat described previously), and are comparable to those of a compact commercial “black box” potentiostat. Likewise, in head-to-head tests, DStat’s potentiometric precision is similar to that of a commercial pH meter. Most importantly, the versatility of DStat was demonstrated through integration with the open-source DropBot digital microfluidics platform. In sum, we propose that DStat is a valuable contribution to the “open source” movement in analytical science, which is allowing users to adapt their tools to their experiments rather than alter their experiments to be compatible with their tools. PMID:26510100

  10. DStat: A Versatile, Open-Source Potentiostat for Electroanalysis and Integration.

    PubMed

    Dryden, Michael D M; Wheeler, Aaron R

    2015-01-01

    Most electroanalytical techniques require the precise control of the potentials in an electrochemical cell using a potentiostat. Commercial potentiostats function as "black boxes," giving limited information about their circuitry and behaviour which can make development of new measurement techniques and integration with other instruments challenging. Recently, a number of lab-built potentiostats have emerged with various design goals including low manufacturing cost and field-portability, but notably lacking is an accessible potentiostat designed for general lab use, focusing on measurement quality combined with ease of use and versatility. To fill this gap, we introduce DStat (http://microfluidics.utoronto.ca/dstat), an open-source, general-purpose potentiostat for use alone or integrated with other instruments. DStat offers picoampere current measurement capabilities, a compact USB-powered design, and user-friendly cross-platform software. DStat is easy and inexpensive to build, may be modified freely, and achieves good performance at low current levels not accessible to other lab-built instruments. In head-to-head tests, DStat's voltammetric measurements are much more sensitive than those of "CheapStat" (a popular open-source potentiostat described previously), and are comparable to those of a compact commercial "black box" potentiostat. Likewise, in head-to-head tests, DStat's potentiometric precision is similar to that of a commercial pH meter. Most importantly, the versatility of DStat was demonstrated through integration with the open-source DropBot digital microfluidics platform. In sum, we propose that DStat is a valuable contribution to the "open source" movement in analytical science, which is allowing users to adapt their tools to their experiments rather than alter their experiments to be compatible with their tools. PMID:26510100

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

    SciTech Connect

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

    2014-03-01

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

  12. A low-cost miniaturized potentiostat for point-of-care diagnosis.

    PubMed

    Cruz, Andres Felipe Diaz; Norena, Nicolas; Kaushik, Ajeet; Bhansali, Shekhar

    2014-12-15

    This paper presents a novel approach of using a miniaturized potentiostat (M-P) chip (LMP91000) to perform full range cyclic voltammetry (CV) measurements for the detection of biomarkers. The LMP91000 evaluation board was reconfigured to perform three-electrode CV measurements in order to achieve electrochemical cortisol immunosensing. The microelectrodes for cortisol estimation were fabricated by immobilizing monoclonal anti-cortisol antibody (Anti-M-Cab) onto self-assembled monolayer (SAM) modified Au microelectrodes. The results obtained using the M-P were compared to those obtained using a conventional potentiostat. The M-P was successful in measuring cortisol levels in the range of pM. The outcomes of the studies suggest that M-P can effectively perform biochemical measurements on three electrode systems, enabling the development of miniature systems for point-of-care (POC) diagnosis. PMID:25016332

  13. CMOS neurotransmitter microarray: 96-channel integrated potentiostat with on-die microsensors.

    PubMed

    Nazari, Meisam Honarvar; Mazhab-Jafari, Hamed; Leng, Lian; Guenther, Axel; Genov, Roman

    2013-06-01

    A 8 × 12 array of integrated potentiostats for on-CMOS neurotransmitter imaging is presented. Each potentiostat channel measures bidirectional redox currents proportional to the concentration of a neurochemical. By combining the current-to-frequency and the single-slope analog-to-digital converter (ADC) architectures a total linear dynamic range of 95 dB is achieved. A 3.8 mm × 3.1 mm prototype fabricated in a 0.35 μm standard CMOS technology was integrated with flat and 3D on-die gold microelectrodes and an on-chip microfluidic network. It is experimentally validated in in-situ recording of neurotransmitter dopamine. PMID:23853333

  14. Use of a mobile phone for potentiostatic control with low cost paper-based microfluidic sensors.

    PubMed

    Delaney, Jacqui L; Doeven, Egan H; Harsant, Anthony J; Hogan, Conor F

    2013-08-01

    By exploiting its ability to play sounds, a mobile phone with suitable software installed can serve the basic functions of a potentiostat in controlling an applied potential to oxidise ECL-active molecules, while the resultant photonic signal is monitored using the camera in video mode. In combination with paper microfluidic sensors this opens significant new possibilities for low-cost, instrument-free sensing. PMID:23870409

  15. A cost-effective and field-ready potentiostat that poises subsurface electrodes to monitor bacterial respiration.

    PubMed

    Friedman, Elliot S; Rosenbaum, Miriam A; Lee, Alexander W; Lipson, David A; Land, Bruce R; Angenent, Largus T

    2012-02-15

    Here, we present the proof-of-concept for a subsurface bioelectrochemical system (BES)-based biosensor capable of monitoring microbial respiration that occurs through exocellular electron transfer. This system includes our open-source design of a three-channel microcontroller-unit (MCU)-based potentiostat that is capable of chronoamperometry, which laboratory tests showed to be accurate within 0.95 ± 0.58% (95% Confidence Limit) of a commercial potentiostat. The potentiostat design is freely available online: http://angenent.bee.cornell.edu/potentiostat.html. This robust and field-ready potentiostat, which can withstand temperatures of -30°C, can be manufactured at relatively low cost ($600), thus, allowing for en-masse deployment at field sites. The MCU-based potentiostat was integrated with electrodes and a solar panel-based power system, and deployed as a biosensor to monitor microbial respiration in drained thaw lake basins outside Barrow, AK. At three different depths, the working electrode of a microbial three-electrode system (M3C) was maintained at potentials corresponding to the microbial reduction of iron(III) compounds and humic acids. Thereby, the working electrode mimics these compounds and is used by certain microbes as an electron acceptor. The sensors revealed daily cycles in microbial respiration. In the medium- and deep-depth electrodes the onset of these cycles followed a considerable increase in overall activity that corresponded to those soils reaching temperatures conducive to microbial activity as the summer thaw progressed. The BES biosensor is a valuable tool for studying microbial activity in situ in remote environments, and the cost-efficient design of the potentiostat allows for wide-scale use in remote areas. PMID:22209069

  16. Potentiostatic and ac impedance studies of the hydrogen electrodes used in Ni/H2 batteries

    NASA Technical Reports Server (NTRS)

    Le Helloco, Jean-Guy; Bojkov, Hristo; Parthasarathy, Arvind; Srinivasan, Supramaniam; Appleby, A. J.

    1992-01-01

    In a study of electrode activity for hydrogen evolution and hydrogen ionization, knowledge of the detailed kinetics and of the surface coverage by adsorbed hydrogen is essential. In the Ni/H2 battery, the hydrogen electrode is subjected to high hydrogen pressure; elucidation of the variation of kinetic parameters with hydrogen pressure is therefore of interest. Potentiostatic and ac impedance spectroscopic techniques were used in the present study. The equivalent circuit of the reaction, the kinetic parameters, and their pressure dependence have been determined.

  17. A compact hybrid-multiplexed potentiostat for real-time electrochemical biosensing applications.

    PubMed

    Ramfos, Ioannis; Vassiliadis, Nikolaos; Blionas, Spyridon; Efstathiou, Konstantinos; Fragoso, Alex; O'Sullivan, Ciara K; Birbas, Alexios

    2013-09-15

    The architecture and design of a compact, multichannel, hybrid-multiplexed potentiostat for performing electrochemical measurements on continuously-biased electrode arrays is presented. The proposed architecture utilises a combination of sequential and parallel measurements, to enable high performance whilst keeping the system low-cost and compact. The accuracy of the signal readout is maintained by following a special multiplexing approach, which ensures the continuous biasing of all the working electrodes of an array. After sampling the results, a digital calibration technique factors out errors from component inaccuracies. A prototype printed circuit board (PCB) was designed and built using off-the-shelf components for the real-time measurement of the amperometric signal of 48 electrodes. The operation and performance of the PCB was evaluated and characterised through a wide range of testing conditions, where it exhibited high linearity (R(2)>0.999) and a resolution of 400pA. The effectiveness of the proposed multiplexing scheme is demonstrated through electrochemical tests using KCl and [Fe(CN)6](3-) in KCl solutions. The applicability of the prototype multichannel potentiostat is also demonstrated using real biosensors, which were applied to the detection of IgA antibodies. PMID:23624017

  18. Purification of supporting electrolyte by a moderate current pre-electrolysis potentiostat

    SciTech Connect

    Brown, B.B.; Paul, D.W.; Ridgway, T.H.; Heineman, W.R.

    1986-01-01

    Anodic stripping voltammetry (ASV) is a well known technique for determining ppb levels of metal ions in environmental samples. One problem in the determination of metal ions at this low concentration level is the contribution of comparatively large amounts of metal ions originating from supporting electrolyte that is added to the sample and used to prepare standards. Pre-electrolysis has been found to reduce the heavy metal content in supporting electrolyte solutions to a few ppb. A moderate current, low cost, potentiostat and an electrochemical cell have been developed for the purification of supporting electrolytes by pre-electrolysis. It provides the moderate current needed at the start of the electrolysis especially during double layer charging as well as the small faradaic current needed through the duration of the electrolysis.

  19. Distinguishing between chi and sigma phases in duplex stainless steels using potentiostatic etching

    SciTech Connect

    Jackson, E.M.L.E.M.; Visser, P.E. de . Physical Metallurgy Div.); Cornish, L.A. )

    1993-12-01

    A color interference film etching technique based on the principle of potentiostatic etching has been developed to distinguish, by optical metallography, between Cr-rich sigma and Mo-rich chi phases as well as with simultaneous identification of the ferrite and austenite phases in duplex stainless steels. The optical metallography results are confirmed by semiquantitative energy dispersive spectrometry analysis and back-scattered electron imaging. The technique is relatively simple and rapid, and makes use of low voltages and a hot etchant. Results have shown distinctively the sigma, chi, ferrite, and austenite phases, and enable observation of the microstructural development, morphology, and kinetics of formation of the phases in duplex alloys. The method, by giving excellent color contrast between sigma and chi, also facilitates quantitative image analysis of the sigma and chi volume fractions.

  20. CheapStat: An Open-Source, “Do-It-Yourself” Potentiostat for Analytical and Educational Applications

    PubMed Central

    Rowe, Aaron A.; Bonham, Andrew J.; White, Ryan J.; Zimmer, Michael P.; Yadgar, Ramsin J.; Hobza, Tony M.; Honea, Jim W.; Ben-Yaacov, Ilan; Plaxco, Kevin W.

    2011-01-01

    Although potentiostats are the foundation of modern electrochemical research, they have seen relatively little application in resource poor settings, such as undergraduate laboratory courses and the developing world. One reason for the low penetration of potentiostats is their cost, as even the least expensive commercially available laboratory potentiostats sell for more than one thousand dollars. An inexpensive electrochemical workstation could thus prove useful in educational labs, and increase access to electrochemistry-based analytical techniques for food, drug and environmental monitoring. With these motivations in mind, we describe here the CheapStat, an inexpensive (<$80), open-source (software and hardware), hand-held potentiostat that can be constructed by anyone who is proficient at assembling circuits. This device supports a number of potential waveforms necessary to perform cyclic, square wave, linear sweep and anodic stripping voltammetry. As we demonstrate, it is suitable for a wide range of applications ranging from food- and drug-quality testing to environmental monitoring, rapid DNA detection, and educational exercises. The device's schematics, parts lists, circuit board layout files, sample experiments, and detailed assembly instructions are available in the supporting information and are released under an open hardware license. PMID:21931613

  1. Fabrication of triazinedithiol functional polymeric nanofilm by potentiostatic polymerization on aluminum surface

    NASA Astrophysics Data System (ADS)

    Wang, Fang; Wang, Yabin; Li, Yanni; Wang, Qian

    2011-01-01

    The functional polymeric nanofilm of 6-(N-allyl-1,1,2,2-tetrahydroperfluorodecyl)amino-1,3,5-triazine-2,4-dithiol monosodium (AF17N) was prepared on pure aluminum surface by potentiostatic polymerization at different potentials. The thickness and weight of polymeric nanofilm increased proportionally to electro-polymerization potential following linear equation. The chemical structure of nanofilm was characterized by Fourier transform-infrared (FT-IR) spectroscopy and X-ray photoelectron spectroscopy (XPS). Adsorption peaks in FT-IR and C1s, N1s, S2p, F1s and Al2p peaks in XPS spectra indicated that the polymeric nanofilm was poly(6-(N-allyl-1,1,2,2-tetrahydroperfluorodecyl)amino-1,3,5-triazine-2,4-disulfide) (PAF17). The morphologies of polymeric nanofilm were also observed by atomic force microscopy (AFM). All the results showed that the optimal electro-polymerization potential and time were 8 V and 20 s, respectively. Uniform and compact nanofilm of PAF17 could be obtained under these conditions. It is expected that this technique will be applied in the preparation of lubricating, dielectric and hydrophobic surface on aluminum substrate.

  2. Reprint of: Use of a mobile phone for potentiostatic control with low cost paper-based microfluidic sensors.

    PubMed

    Delaney, Jacqui L; Doeven, Egan H; Harsant, Anthony J; Hogan, Conor F

    2013-11-25

    By exploiting its ability to play sounds, a mobile phone with suitable software installed can serve the basic functions of a potentiostat in controlling an applied potential to oxidise ECL-active molecules, while the resultant photonic signal is monitored using the camera in video mode. In combination with paper microfluidic sensors this opens significant new possibilities for low-cost, instrument-free sensing. PMID:24216205

  3. Anomalous codeposition of Fe-Ni alloys and Fe-Ni-SiO{sub 2} composites under potentiostatic conditions: Experimental study and mathematical model

    SciTech Connect

    Ramasubramanian, M.; Popova, S.N.; Popov, B.N.; White, R.E.; Yin, K.M.

    1996-07-01

    A mathematical model has been developed to describe the electrodeposition of Fe-Ni alloys and Fe-Ni-SiO{sub 2} composites under potentiostatic conditions. This model can be used to predict the polarization behavior, partial current densities, and alloy composition of each of the components as a function of the applied potential. Fe-Ni-SiO{sub 2} samples were deposited on platinum rotating disk electrodes from sulfate electrolytes under potentiostatic conditions, and the results obtained were compared to the model. The model predictions were found to agree well with the experimental observations for the Fe-Ni and Fe-Ni-SiO{sub 2} systems.

  4. Direct observation of hydration of TiO 2 on Ti using electrochemical AFM: freely corroding versus potentiostatically held

    NASA Astrophysics Data System (ADS)

    Bearinger, Jane P.; Orme, Christine A.; Gilbert, Jeremy L.

    2001-10-01

    Hydration of titanium/titanium oxide surfaces under freely corroding and potentiostatically held conditions has been characterized using electrochemical atomic force microscopy (EC AFM). In contrast to conventional high vacuum techniques, AFM enables measurement of morphological surface structure in the in situ hydrated state. Electrochemical probes in the imaging environment further enable acquisition of electrical characteristics during AFM imaging. Experiments were performed on etched, electropolished commercially pure titanium. As noted by direct observation and corroborated by power spectral density (Fourier analysis) measurements, oxide domes cover the titanium surface and grow laterally during hydration. Applied potential altered the growth rate. Under open circuit potential conditions, growth proceeded approximately six times faster than under a -1 V applied voltage ( 1098±52 nm2/ min ± versus 184.84±19 nm2/min). Film growth increased electrical resistance and lowered interfacial capacitance based on step polarization impedance spectroscopy tests.

  5. A potentiostat featuring an integrator transimpedance amplifier for the measurement of very low currents—Proof-of-principle application in microfluidic separations and voltammetry

    NASA Astrophysics Data System (ADS)

    Koutilellis, G. D.; Economou, A.; Efstathiou, C. E.

    2016-03-01

    This work reports the design and construction of a novel potentiostat which features an integrator transimpedance amplifier as a current-monitoring unit. The integration approach addresses the limitations of the feedback resistor approach used for current monitoring in conventional potentiostat designs. In the present design, measurement of the current is performed by a precision switched integrator transimpedance amplifier operated in the dual sampling mode which enables sub-pA resolution. The potentiostat is suitable for measuring very low currents (typical dynamic range: 5 pA-4.7 μA) with a 16 bit resolution, and it can support 2-, 3- and 4-electrode cell configurations. Its operation was assessed by using it as a detection module in a home-made capillary electrophoresis system for the separation and amperometric detection of paracetamol and p-aminophenol at a 3-electrode microfluidic chip. The potential and limitations of the proposed potentiostat to implement fast potential-scan voltammetric techniques were demonstrated for the case of cyclic voltammetry.

  6. A potentiostat featuring an integrator transimpedance amplifier for the measurement of very low currents-Proof-of-principle application in microfluidic separations and voltammetry.

    PubMed

    Koutilellis, G D; Economou, A; Efstathiou, C E

    2016-03-01

    This work reports the design and construction of a novel potentiostat which features an integrator transimpedance amplifier as a current-monitoring unit. The integration approach addresses the limitations of the feedback resistor approach used for current monitoring in conventional potentiostat designs. In the present design, measurement of the current is performed by a precision switched integrator transimpedance amplifier operated in the dual sampling mode which enables sub-pA resolution. The potentiostat is suitable for measuring very low currents (typical dynamic range: 5 pA-4.7 μA) with a 16 bit resolution, and it can support 2-, 3- and 4-electrode cell configurations. Its operation was assessed by using it as a detection module in a home-made capillary electrophoresis system for the separation and amperometric detection of paracetamol and p-aminophenol at a 3-electrode microfluidic chip. The potential and limitations of the proposed potentiostat to implement fast potential-scan voltammetric techniques were demonstrated for the case of cyclic voltammetry. PMID:27036788

  7. The use of a new potentiostat/coulometer in the controlled-potential coulometric determination of plutonium

    SciTech Connect

    Mendoza, P.G. Jr.; Temer, D.J.; Jackson, D.D.

    1993-10-01

    We evaluated a PAR 273 potentiostat and PAR 279 coulometer using iron as a stand-in for plutonium. Over 400 tuns consisting of electrical checks, blanks, and iron solutions were made. Manual operation of the instrumentation produced precisions better than 0.1%. Computer control of the instrumentation produced precisions better than 0.1%. Computer control of the instrumentation using a PC and a program written in QuickBASIC produced precisions of about 0.12%. The computer program automatically set up and controlled the instrumentation and recorded the data. The potentionstat`s current autoranging function caused erractic coulometer results. Use of the PAR 273`s low-pass filter (LPF) removed the amperometric end-point current noise, but it also biased the current. The PAR 273A`s LPF filtered the noise without introducing a bias. The coulometer functions, such as current integration and communication interface, occasionally locked up after a current overrange condition. The occasional procedural error revealed that the potentionstat`s ability to produce >1 A current can ruin the coulometer`s impact circuitry, which is protected up to 0.2 A for current ranges <1 A.

  8. Re-passivation Potential of Alloy 22 in Chloride plus Nitrate Solutions using the Potentiodynamic-Galvano-static-Potentiostatic Method

    SciTech Connect

    Evans, Kenneth J.; Rebak, Raul B.

    2007-07-01

    In general, the susceptibility of Alloy 22 to suffer crevice corrosion is measured using the Cyclic Potentiodynamic Polarization (CPP) technique. This is a fast technique that gives rather accurate and reproducible values of re-passivation potential (ER1) in most cases. In the fringes of susceptibility, when the environment is not highly aggressive, the values of re-passivation potential using the CPP technique may not be highly reproducible, especially because the technique is fast. To circumvent this, the re-passivation potential of Alloy 22 was measured using a slower method that combines Potentiodynamic-Galvano-static-Potentiostatic steps (called here the Tsujikawa-Hisamatsu Electrochemical or THE method). The THE method applies the charge to the specimen in a more controlled way, which may give more reproducible re-passivation potential values, especially when the environment is not aggressive. The values of re-passivation potential of Alloy 22 in sodium chloride plus potassium nitrate solutions were measured using the THE and CPP methods. Results show that both methods yield similar values of re-passivation potential, especially under aggressive conditions. (authors)

  9. Integrated potentiostat for electrochemical sensing of urinary 3-hydroxyanthranilic acid with molecularly imprinted poly(ethylene-co-vinyl alcohol).

    PubMed

    Huang, Chun-Yueh; O'Hare, Danny; Chao, I-Jen; Wei, Hung-Wei; Liang, Yi-Fan; Liu, Bin-Da; Lee, Mei-Hwa; Lin, Hung-Yin

    2015-05-15

    Changing demographics, the rise of personalized medicine and increased identification of biomarkers for diagnosis and management of chronic disease have increased the demand for portable bioanalytical instrumentation and point-of-care. The recent development of molecularly imprinted polymers enables production of low cost and highly stable sensing chips; however, the commercially available and full functional instruments employed for electrochemical analysis have shortcomings in actual homecare applications. In this work, integrated circuits (ICs) for monolithic implementation of voltammeter potentiostat with a large dynamic current range (5 nA to 1.2 mA) and short conversion time (10 ms) were fabricated in a 0.35 μm complementary metal-oxide-semiconductor (CMOS) process. The new instrumentation was tested with molecular imprinted sensors for 3-hydroxyanthranilic acid (3HAA) in urine. The sensor consisted of molecular imprinted of poly(ethylene-co-vinyl alcohol)s (abbreviated as EVALs) for implementation in a flow injection analysis system. The EVAL containing 32 ethylene mol% had the highest imprinting effectiveness for the target molecules. Fit-for-purpose figures of merit were achieved with a limit-of-detection (LOD) of 3.06 pg/mL. The measurements obtained in real undiluted urine samples fell within the reference concentration range of 50-550 ng/mL. PMID:25175746

  10. Comparative electron microscopy (SEM) examination of Fe, Au, and Zn electrode surfaces polarized in different regions of potentiostatic E/I behavior

    SciTech Connect

    Podesta, J.J.; Arvia, A.J.; Piatti, R.C.V.

    1982-12-01

    The surface morphology of some metals (Fe, Au, and Zn) after potentiostatic polarization was studied through SEM examination. The following electrochemical systems were investigated at 25C: (1) Fe/1 M H/sub 2/SO/sub 4/; (2) Au/1 M HCl; and (3) Zn/2 M NaOH. The polarization potentials were chosen in the active dissolution region, in the passivity region, and in the potential range where periodic oscillations of the anode current are observed. The changes in the morphologies of attack on the various metals were related to the film forming species and of anion adsorption.

  11. Comparison of Galvanic Currents Generated Between Different Combinations of Orthodontic Brackets and Archwires Using Potentiostat: An In Vitro Study

    PubMed Central

    Nayak, Rabindra S; Shafiuddin, Bareera; Pasha, Azam; Vinay, K; Narayan, Anjali; Shetty, Smitha V

    2015-01-01

    Background: Technological advances in wire selection and bracket design have led to improved treatment efficiency and allowed longer time intervals between appliance adjustments. The wires remain in the mouth for a longer duration and are subjected to electrochemical reactions, mechanical forces of mastication and generalized wear. These cause different types of corrosion. This study was done to compare the galvanic currents generated between different combinations of brackets and archwires commonly used in orthodontic practices. Materials and Methods: The materials used for the study included different commercially available orthodontic archwires and brackets. The galvanic current generated by individual materials and different combinations of these materials was tested and compared. The orthodontic archwires used were 0.019″ × 0.025″ heat-activated nickel-titanium (3M Unitek), 0.019″ × 0.025″ beta-titanium (3M Unitek) and 0.019″ × 0.025″ stainless steel (3M Unitek). The orthodontic brackets used were 0.022″ MBT laser-cut (Victory Series, 3M Unitek) and metal-injection molded (Leone Company) maxillary central incisor brackets respectively. The ligature wire used for ligation was 0.009″ stainless steel ligature (HP Company). The galvanic current for individual archwires, brackets, and the different bracket-archwire-ligature combinations was measured by using a Potentiostat machine. The data were generated using the Linear Sweep Voltammetry and OriginPro 8.5 Graphing and Data Analysis Softwares. The study was conducted in two phases. Phase I comprised of five groups for open circuit potential (OCP) and galvanic current (I), whereas Phase II comprised of six groups for galvanic current alone. Results: Mean, standard deviation and range were computed for the OCP and galvanic current (I) values obtained. Results were subjected to statistical analysis through ANOVA. In Phase I, higher mean OCP was recorded in stainless steel archwire, followed by beta-titanium archwire, heat-activated nickel titanium archwire, laser-cut bracket and metal-injection molded bracket, respectively. The difference in mean OCP recorded among the groups was found to be statistically significant in aerated phosphate buffered saline solution. The galvanic current (I) for metal-injection molded stainless steel brackets showed significantly higher values than all the other materials. Phase II results suggested that, in the couples formed by the archwire-bracket-ligature combinations, the bracket had more important contribution to the total galvanic current generated, since there were significant differences between galvanic current among the 2 brackets tested but not among the 3 wires. The galvanic current of the metal-injection molded bracket was significantly higher than that of laser-cut bracket. Highest mean current (I) was recorded in metal-injection molded bracket when used with heat-activated nickel titanium archwire while lowest mean current (I) was recorded in laser-cut bracket when used with beta-titanium archwire. Conclusion: The present study concluded that the bracket emerged to be the most important factor in determining the galvanic current (I). Higher mean current (I) was recorded in metal-injection molded bracket compared to laser-cut bracket. Among the three archwires, higher mean current (I) was recorded in heat-activated nickel-titanium, followed by stainless-steel and beta-titanium respectively. When coupled together; highest mean current (I) was recorded in metal-injection molded bracket when used with heat-activated nickel titanium archwire while lowest mean current (I) was recorded in laser-cut bracket when used with beta-titanium archwire. PMID:26229367

  12. Investigation of the growth and local stoichiometric point group symmetry of titania nanotubes during potentiostatic anodization of titanium in phosphate electrolytes

    NASA Astrophysics Data System (ADS)

    Cummings, F. R.; Muller, T. F. G.; Malgas, G. F.; Arendse, C. J.

    2015-10-01

    Potentiostatic anodization of commercially pure, 50 μm-thick titanium (Ti) foil was performed in aqueous, phosphate electrolytes at increasing experimental timeframes at a fixed applied potential for the synthesis of titania nanotube arrays (TNAs). High resolution scanning electron microscopy images, combined with energy dispersive spectroscopy and x-ray diffraction spectra reveal that anodization of the Ti foil in a 1 M NaF+0.5 M H3PO4 electrolyte for 4 h yields a titanate surface with pore diameters ranging between 100 and 500 nm. The presence of rods on the Ti foil surface with lengths exceeding 20 μm and containing high concentrations of phosphor on the exterior was also detected at these conditions, along with micro-sized coral reef-like titanate balls. We propose that the formation of these structures play a major role during the anodization process and impedes nanotube growth during the anodization process. High spatially resolved scanning transmission electron microscopy-electron energy loss spectroscopy (STEM-EELS) performed along the length of a single anodized TiO2 nanotube reveals a gradual evolution of the nanotube crystallinity, from a rutile-rich bottom to a predominantly anatase TiO2 structure along its length.

  13. Evaluation of in-channel amperometric detection using a dual-channel microchip electrophoresis device and a two-electrode potentiostat for reverse polarity separations

    PubMed Central

    Meneses, Diogenes; Gunasekara, Dulan B.; Pichetsurnthorn, Pann; da Silva, José A. F.; de Abreu, Fabiane C.; Lunte, Susan M.

    2015-01-01

    In-channel amperometric detection combined with dual-channel microchip electrophoresis is evaluated using a two-electrode isolated potentiostat for reverse polarity separations. The device consists of two separate channels with the working and reference electrodes placed at identical positions relative to the end of the channel, enabling noise subtraction. In previous reports of this configuration, normal polarity and a three-electrode detection system were used. In the two-electrode detection system described here, the electrode in the reference channel acts as both the counter and reference. The effect of electrode placement in the channels on noise and detector response was investigated using nitrite, tyrosine, and hydrogen peroxide as model compounds. The effects of electrode material and size and type of reference electrode on noise and the potential shift of hydrodynamic voltammograms for the model compounds were determined. In addition, the performance of two- and three-electrode configurations using Pt and Ag/AgCl reference electrodes was compared. Although the signal was attenuated with the Pt reference, the noise was also significantly reduced. It was found that lower LOD were obtained for all three compounds with the dual-channel configuration compared to single-channel, in-channel detection. The dual-channel method was then used for the detection of nitrite in a dermal microdialysis sample obtained from a sheep following nitroglycerin administration. PMID:25256669

  14. Parallel Recording of Neurotransmitters Release from Chromaffin Cells Using a 10 × 10 CMOS IC Potentiostat Array with On-Chip Working Electrodes

    PubMed Central

    Kim, Brian Namghi; Herbst, Adam D.; Kim, Sung June; Minch, Bradley A.; Lindau, Manfred

    2012-01-01

    Neurotransmitter release is modulated by many drugs and molecular manipulations. We present an active CMOS-based electrochemical biosensor array with high throughput capability (100 electrodes) for on-chip amperometric measurement of neurotransmitter release. The high-throughput of the biosensor array will accelerate the data collection needed to determine statistical significance of changes produced under varying conditions, from several weeks to a few hours. The biosensor is designed and fabricated using a combination of CMOS integrated circuit (IC) technology and a photolithography process to incorporate platinum working electrodes on-chip. We demonstrate the operation of an electrode array with integrated high-gain potentiostats and output time-division multiplexing with minimum dead time for readout. The on-chip working electrodes are patterned by conformal deposition of Pt and lift-off photolithography. The conformal deposition method protects the underlying electronic circuits from contact with the electrolyte that covers the electrode array during measurement. The biosensor was validated by simultaneous measurement of amperometric currents from 100 electrodes in response to dopamine injection, which revealed the time course of dopamine diffusion along the surface of the biosensor array. The biosensor simultaneously recorded neurotransmitter release successfully from multiple individual living chromaffin cells. The biosensor was capable of resolving small and fast amperometric spikes reporting release from individual vesicle secretions. We anticipate that this device will accelerate the characterization of the modulation of neurotransmitter secretion from neuronal and endocrine cells by pharmacological and molecular manipulations of the cells. PMID:23084756

  15. Evaluation of in-channel amperometric detection using a dual-channel microchip electrophoresis device and a two-electrode potentiostat for reverse polarity separations.

    PubMed

    Meneses, Diogenes; Gunasekara, Dulan B; Pichetsurnthorn, Pann; da Silva, José A F; de Abreu, Fabiane C; Lunte, Susan M

    2015-02-01

    In-channel amperometric detection combined with dual-channel microchip electrophoresis is evaluated using a two-electrode isolated potentiostat for reverse polarity separations. The device consists of two separate channels with the working and reference electrodes placed at identical positions relative to the end of the channel, enabling noise subtraction. In previous reports of this configuration, normal polarity and a three-electrode detection system were used. In the two-electrode detection system described here, the electrode in the reference channel acts as both the counter and reference. The effect of electrode placement in the channels on noise and detector response was investigated using nitrite, tyrosine, and hydrogen peroxide as model compounds. The effects of electrode material and size and type of reference electrode on noise and the potential shift of hydrodynamic voltammograms for the model compounds were determined. In addition, the performance of two- and three-electrode configurations using Pt and Ag/AgCl reference electrodes was compared. Although the signal was attenuated with the Pt reference, the noise was also significantly reduced. It was found that lower LOD were obtained for all three compounds with the dual-channel configuration compared to single-channel, in-channel detection. The dual-channel method was then used for the detection of nitrite in a dermal microdialysis sample obtained from a sheep following nitroglycerin administration. PMID:25256669

  16. Parallel recording of neurotransmitters release from chromaffin cells using a 10×10 CMOS IC potentiostat array with on-chip working electrodes.

    PubMed

    Kim, Brian N; Herbst, Adam D; Kim, Sung J; Minch, Bradley A; Lindau, Manfred

    2013-03-15

    Neurotransmitter release is modulated by many drugs and molecular manipulations. We present an active CMOS-based electrochemical biosensor array with high throughput capability (100 electrodes) for on-chip amperometric measurement of neurotransmitter release. The high-throughput of the biosensor array will accelerate the data collection needed to determine statistical significance of changes produced under varying conditions, from several weeks to a few hours. The biosensor is designed and fabricated using a combination of CMOS integrated circuit (IC) technology and a photolithography process to incorporate platinum working electrodes on-chip. We demonstrate the operation of an electrode array with integrated high-gain potentiostats and output time-division multiplexing with minimum dead time for readout. The on-chip working electrodes are patterned by conformal deposition of Pt and lift-off photolithography. The conformal deposition method protects the underlying electronic circuits from contact with the electrolyte that covers the electrode array during measurement. The biosensor was validated by simultaneous measurement of amperometric currents from 100 electrodes in response to dopamine injection, which revealed the time course of dopamine diffusion along the surface of the biosensor array. The biosensor simultaneously recorded neurotransmitter release successfully from multiple individual living chromaffin cells. The biosensor was capable of resolving small and fast amperometric spikes reporting release from individual vesicle secretions. We anticipate that this device will accelerate the characterization of the modulation of neurotransmitter secretion from neuronal and endocrine cells by pharmacological and molecular manipulations of the cells. PMID:23084756

  17. In vivo potentiostatic studies at the electrode tissue interface: filter properties of the monophasic action potential (Ag/AgCl) electrode in living rat heart.

    PubMed

    Chou, H A; Ovadia, M; Moskowitz, M; Zavitz, D H

    2000-03-01

    The monophasic action potential (Franz) catheter is regarded as the criterion standard for high fidelity recording of a class of physiological signals. However, its signal modulation characteristics have never been reported. Broadband impedance spectroscopy was performed in perfused living rat heart in a three-electrode potentiostatic configuration to determine the filtering characteristics of the MAP and model Ag/AgCl electrode-tissue interfaces. The filter transfer function H(f) (attenuation [dB] vs log(f) [log(Hz)]) was derived for the frequency range 10 Hz-10(6) Hz. As a filter, the MAP interface is characterized by two ranges of filtering behavior. At high frequency the MAP interface is a high-pass filter with passband frequency 54 kHz-549 kHz (median 321 kHz) and with -3 dB cutoff points ranging from 10 kHz to 302 kHz. In this high frequency range the transfer function is characterized by decreasing attenuation per decade. However, in the lower frequency range relevant to physiological signals (the monophasic action potential, 0.1-40 Hz), it is a severely attenuating nondiodic high-pass filter element with an average attenuation of 16.87 dB relative to passband. In this physiological range, rolloff is nonlinear with increasing attenuation per decade. While the MAP electrode and model Ag/AgCl electrodes are high-pass filters with robust transfer functions for high frequency signals in the living heart, the attenuation of signals in a frequency range relevant to in vivo physiological recording imparts extreme attenuation that may distort physiological signals unpredictably. This disadvantage may be mitigated by amplitude scaling to a calibrated pure tone signal within the physiological frequency band to recover a reproducible signal. PMID:10750142

  18. Conversion of an Agilent Chip Cube System and Adaptation of a ROXY EC Potentiostat for the Analysis of Proteolytic and Non-Proteolytic Protein Samples on a Thermo Finnigan LTQ-FT Ultra Mass Spectrometer.

    PubMed Central

    Crot, C.; Helseth, L.; Xu, H.; Davis, R.; Schilling, A.

    2010-01-01

    RP-48 High resolution, high mass accuracy analysis of peptide digests and proteins using hybrid instruments such as the Thermo Finnigan LTQ-FT Ultra instrument allow for faster unambiguous computer identification of proteins from peptide digests, accurate measurement of intact protein MW and detection of post translational modifications by top down methods and the use of auxiliary dissociation methods such as ECD to study disulfide bonds and crosslinked peptides as well as post-translational modifications such as phosphorylation. User demand for these instruments remains high in shared facilities like ours and efforts are always being made to improve sample throughput to increase instrument availability. Several vendors have released microfluidic based integrated chromatographic systems in the last few years that allow for relatively easy use in nanospray mode along with reductions in delay volumes and significant improvement in sample throughput and sensitivity. The current work reports on the successful integration of one such system, the Agilent Chip Cube system, originally designed to work only on MS instruments from that manufacturer, so that it will function routinely on the LTQ-FT Ultra MS. Using the chip cube's nanocolumn cartridge “chips”, our facility has been able to significantly shorten runtimes for digest based analyses of simple and complex fractionated samples while obtaining excellent peptide detection using smaller sample injection volumes. Details of the adaptation will be provided and examples will be shown using data from both CID and ECD based proteolytic workflows. In addition, we will present data generated using an online electrochemical potentiostat, the ROXY EC system, along with the chip cube on the LTQ FT Ultra allowing the detection of electrochemically generated peptide fragments from intact proteins as an adjunct/replacement for proteolysis in specific analytical problems where the use of nano-LC/MS/MS proteolytic analysis is normally required due to low picomolar and femtomolar protein levels.

  19. Potentiostatic deposition of DNA for scanning probe microscopy.

    PubMed Central

    Lindsay, S M; Tao, N J; DeRose, J A; Oden, P I; Lyubchenko YuL; Harrington, R E; Shlyakhtenko, L

    1992-01-01

    We describe a procedure for reversible adsorption of DNA onto a gold electrode maintained under potential control. The adsorbate can be imaged by scanning probe microscopy in situ. Quantitative control of a molecular adsorbate for microscopy is now possible. We found a potential window (between 0 and 180 mV versus a silver wire quasi reference) over which a gold (111) surface under phosphate buffer is positively charged, but is not covered with a dense adsorbate. When DNA is present in these conditions, molecules adsorb onto the electrode and remain stable under repeated scanning with a scanning tunneling microscope (STM). They become removed when the surface is brought to a negative charge. When operated at tunnel currents below approximately 0.4 nA, the STM yields a resolution of approximately 1 nm, which is better than can be obtained with atomic force microscopy (AFM) at present. We illustrate this procedure by imaging a series of DNA molecules made by ligating a 21 base-pair oligonucleotide. We observed the expected series of fragment lengths but small fragments are adsorbed preferentially. Images FIGURE 3 FIGURE 4 FIGURE 5 FIGURE 6 FIGURE 7 FIGURE 8 FIGURE 9 FIGURE 10 FIGURE 11 PMID:1617139

  20. Intelligent potentiostat for identification of heavy metals in situ

    NASA Astrophysics Data System (ADS)

    Christidis, K.; Gow, K.; Robertson, P.; Pollard, P.

    2006-01-01

    This article presents a low-cost portable electrochemical instrument capable of on-site identification of heavy metals. The instrument acquires metal-specific voltage and current signals by the application of differential pulse anodic stripping voltammetry. This technique enhances the analytical current and rejects the background current, resulting in a higher signal-to-noise ratio for a better detection limit. The identification of heavy metals is based on an intelligent machine-based method using a multilayer perceptron neural network consisting of three layers of neurons. The neural network is implemented using a 16 bit microcontroller. The system is developed for use in the field in order to avoid expensive and time-consuming procedures and can be used in a variety of situations to help environmental assessment and control.

  1. Determination of the Crevice Repassivation Potential of Alloy 22 By a Potentiodynamic-Galvanostatic-Potentiostatic Method

    SciTech Connect

    K. Evans; L. Wong; R. Rebak

    2004-06-01

    Alloy 22 (N06022) is a nickel-based alloy highly resistant to corrosion. In some aggressive conditions of high chloride concentration, temperature and applied potential, Alloy 22 may suffer crevice corrosion, a form of localized corrosion. There are several electrochemical methods that can be used to determine localized corrosion in metallic alloys. One of the most popular for rapid screening is the cyclic potentiodynamic polarization (CPP). This work compares the results obtained by measuring the localized corrosion resistance of Alloy 22 using both CPP and the more cumbersome Tsujikawa-Hisamatsu Electrochemical (THE) method. The electrolytes used were 1 M NaCl and 5 M CaCl{sub 2}, both at 90 C. Results show that similar repassivation potentials were obtained for Alloy 22 using both methods. That is, in cases where localized corrosion is observed using the fast CPP method, there is no need to use THE method since it takes ten times longer to obtain comparable results in spite of the mode of corrosion attack is different in the tested specimens.

  2. Study of Metal-NH[subscript 3] Interfaces (Metal= Cu, Ni, Ag) Using Potentiostatic Curves

    ERIC Educational Resources Information Center

    Nunes, Nelson; Martins, Angela; Leitao, Ruben Elvas

    2007-01-01

    Experiment is conducted to determine the kinetic parameters of metal-solution interfaces. During the experiment the kinetic parameters for the interfaces Cu-NH[subscript 3], Ag-NH[subscript 3] and Ni-NH[subscript 3] is easily determined.

  3. Attofarad resolution potentiostat for electrochemical measurements on nanoscale biomolecular interfacial systems.

    PubMed

    Carminati, Marco; Ferrari, Giorgio; Sampietro, Marco

    2009-12-01

    We present an instrument that enables electrochemical measurements (cyclic voltammetry, impedance tracking, and impedance spectroscopy) on submicrometric samples. The system features a frequency range from dc to 1 MHz and a current resolution of 10 fA for a measurement time of 1 s, giving a sensitivity of few attofarads in terms of measurable capacitance with an applied voltage of only 100 mV. These performances are obtained using a low-noise wide-bandwidth integrator/differentiator stage to sense the input current and a modular approach to minimize the effect of input stray capacitances. A digitally implemented lock-in filter optimally extracts the impedance of the sample, providing time tracking and spectroscopy operating modes. This computer-based and flexible instrument is well suited for characterizing and tracking the electrical properties of biomolecules kept in the physiological solution down to the nanoscale. PMID:20059158

  4. CONTROLLED ENVIRONMENT POTENTIOSTAT TO STUDY SOLID-AQUEOUS SYSTEMS. (R825549C051)

    EPA Science Inventory

    The perspectives, information and conclusions conveyed in research project abstracts, progress reports, final reports, journal abstracts and journal publications convey the viewpoints of the principal investigator and may not represent the views and policies of ORD and EPA. Concl...

  5. Attofarad resolution potentiostat for electrochemical measurements on nanoscale biomolecular interfacial systems

    NASA Astrophysics Data System (ADS)

    Carminati, Marco; Ferrari, Giorgio; Sampietro, Marco

    2009-12-01

    We present an instrument that enables electrochemical measurements (cyclic voltammetry, impedance tracking, and impedance spectroscopy) on submicrometric samples. The system features a frequency range from dc to 1 MHz and a current resolution of 10 fA for a measurement time of 1 s, giving a sensitivity of few attofarads in terms of measurable capacitance with an applied voltage of only 100 mV. These performances are obtained using a low-noise wide-bandwidth integrator/differentiator stage to sense the input current and a modular approach to minimize the effect of input stray capacitances. A digitally implemented lock-in filter optimally extracts the impedance of the sample, providing time tracking and spectroscopy operating modes. This computer-based and flexible instrument is well suited for characterizing and tracking the electrical properties of biomolecules kept in the physiological solution down to the nanoscale.

  6. A potentiostatic study of oxygen transport through poly(2-ethoxyethyl methacrylate-co-2,3-dihydroxypropylmethacrylate) hydrogel membranes.

    PubMed

    Compañ, Vicente; Tiemblo, Pilar; García, F; García, J M; Guzmán, Julio; Riande, Evaristo

    2005-06-01

    The oxygen permeability and diffusion coefficients of hydrogel membranes prepared with copolymers of 2-ethoxyethyl methacrylate (EEMA)/2,3-dihydroxypropylmethacrylate (MAG) with mole fraction of the second monomer in the range between 0 and 0.75 are described. Values of the permeability and diffusion coefficients of oxygen are determined by using electrochemical procedures involving the measurement of the steady-state current in membranes prepared by radical polymerization of the monomers. The results obtained for the transport properties were analyzed taking into account the fractional free volumes, the cohesive energy densities and the glass transition temperatures of the hydrogels. PMID:15626426

  7. An investigation on the optimum corrosion protection potential for minimization of cavitation damage using the potentiostatic method in seawater.

    PubMed

    Kim, Seong-Jong; Jang, Seok-Ki; Park, Jae-Cheul

    2013-08-01

    In this study, we replaced the expensive blade material with an aluminum-bronze alloy that has excellent corrosion resistance and cavitation characteristics and developed the corrosion protection method to improve durability using an electrochemical method. The objective of this study was to identify the electrochemical corrosion protection conditions to minimize cavitation damage due to generating hydrogen gas (2H₂O + 2e⁻ → 2OH⁻ + H₂) by means of hydrogen overvoltage before the impact pressure of the cavity is transferred to the surface. In the constant potential experiment under the cavitation environment, the energy was reflected or cancelled out by collision of the cavities with the hydrogen gas generated by the hydrogen overvoltage. As a result, the optimal corrosion prevention potential in the dynamic state is assumed to be the range of -1.4 to -1.7 V, which is the range at which active polarization took place. PMID:23920179

  8. Aerated Shewanella oneidensis in Continuously-fed Bioelectrochemical Systems for Power and Hydrogen Production

    Technology Transfer Automated Retrieval System (TEKTRAN)

    We studied the effects of aeration of Shewanella oneidensis on potentiostatic current production, iron(III) reduction, hydrogen production in a microbial electrolysis cell, and electric power generation in a microbial fuel cell. The potentiostatic performance of aerated S. oneidensis was considerab...

  9. Electrochemical nitridation of metal surfaces

    SciTech Connect

    Wang, Heli; Turner, John A.

    2015-06-30

    Electrochemical nitridation of metals and the produced metals are disclosed. An exemplary method of electrochemical nitridation of metals comprises providing an electrochemical solution at low temperature. The method also comprises providing a three-electrode potentiostat system. The method also comprises stabilizing the three-electrode potentiostat system at open circuit potential. The method also comprises applying a cathodic potential to a metal.

  10. Electrochemical Microsensors for the Detection of Cadmium(II) and Lead(II) Ions in Plants

    PubMed Central

    Krystofova, Olga; Trnkova, Libuse; Adam, Vojtech; Zehnalek, Josef; Hubalek, Jaromir; Babula, Petr; Kizek, Rene

    2010-01-01

    Routine determination of trace metals in complex media is still a difficult task for many analytical instruments. The aim of this work was to compare three electro-chemical instruments [a standard potentiostat (Autolab), a commercially available miniaturized potentiostat (PalmSens) and a homemade micropotentiostat] for easy-to-use and sensitive determination of cadmium(II) and lead(II) ions. The lowest detection limits (hundreds of pM) for both metals was achieved by using of the standard potentiostat, followed by the miniaturized potentiostat (tens of nM) and the homemade instrument (hundreds of nM). Nevertheless, all potentiostats were sensitive enough to evaluate contamination of the environment, because the environmental limits for both metals are higher than detection limits of the instruments. Further, we tested all used potentiostats and working electrodes on analysis of environmental samples (rainwater, flour and plant extract) with artificially added cadmium(II) and lead(II). Based on the similar results obtained for all potentiostats we choose a homemade instrument with a carbon tip working electrode for our subsequent environmental experiments, in which we analyzed maize and sunflower seedlings and rainwater obtained from various sites in the Czech Republic. PMID:22219663

  11. Electrochemical microsensors for the detection of cadmium(II) and lead(II) ions in plants.

    PubMed

    Krystofova, Olga; Trnkova, Libuse; Adam, Vojtech; Zehnalek, Josef; Hubalek, Jaromir; Babula, Petr; Kizek, Rene

    2010-01-01

    Routine determination of trace metals in complex media is still a difficult task for many analytical instruments. The aim of this work was to compare three electro-chemical instruments [a standard potentiostat (Autolab), a commercially available miniaturized potentiostat (PalmSens) and a homemade micropotentiostat] for easy-to-use and sensitive determination of cadmium(II) and lead(II) ions. The lowest detection limits (hundreds of pM) for both metals was achieved by using of the standard potentiostat, followed by the miniaturized potentiostat (tens of nM) and the homemade instrument (hundreds of nM). Nevertheless, all potentiostats were sensitive enough to evaluate contamination of the environment, because the environmental limits for both metals are higher than detection limits of the instruments. Further, we tested all used potentiostats and working electrodes on analysis of environmental samples (rainwater, flour and plant extract) with artificially added cadmium(II) and lead(II). Based on the similar results obtained for all potentiostats we choose a homemade instrument with a carbon tip working electrode for our subsequent environmental experiments, in which we analyzed maize and sunflower seedlings and rainwater obtained from various sites in the Czech Republic. PMID:22219663

  12. Localized corrosion of mild steel in base solutions containing sodium sulfide. Influence of pH and sodium acetate addition

    SciTech Connect

    Vasquez, D.; Arvia, A.J.; Salvarezza, R.C.; Videla, H.A.

    1984-08-01

    This paper presents a study of the role played by sulfide, hydroxyl, and acetate ions in solution to explain pit initiation and growth on mild steel. Potentiostatic and potentiodynamic techniques described in previous publications were used.

  13. SWEPT-POTENTIAL ELECTROCHEMICAL DETECTOR FOR FLOW STREAMS

    EPA Science Inventory

    An instrument has been designed, constructed, and evaluated for electrochemical measurements in flow streams. The instrument is basically a computer-controlled potentiostat with features that are necessary for measurements in flow streams. These features include real-time graphic...

  14. Apparatus for use in rapid and accurate controlled-potential coulometric analysis

    DOEpatents

    Frazzini, Thomas L.; Holland, Michael K.; Pietri, Charles E.; Weiss, Jon R.

    1981-01-01

    An apparatus for controlled-potential coulometric analysis of a solution includes a cell to contain the solution to be analyzed and a plurality of electrodes to contact the solution in the cell. Means are provided to stir the solution and to control the atmosphere above it. A potentiostat connected to the electrodes controls potential differences among the electrodes. An electronic circuit connected to the potentiostat provides analog-to-digital conversion and displays a precise count of charge transfer during a desired chemical process. This count provides a measure of the amount of an unknown substance in the solution.

  15. Characterization of electrochemically deposited polypyrrole using magnetoelastic material transduction elements

    NASA Technical Reports Server (NTRS)

    Ersoz, Arzu; Ball, J. Christopher; Grimes, Craig A.; Bachas, Leonidas G.

    2002-01-01

    Magnetoelastic alloy films have been used as a working electrode in an electrochemical cell. This material allows magnetic interrogation of electrochemical deposition. This technique was used to monitor the electrochemical deposition of polypyrrole by multisweep (CV) and potentiostatic methods. Since the determination of the mass-sensitive magnetoelastic film's resonance frequency is based on magnetic transduction, an inherent advantage of this method is that it requires no electrical connections other than the working lead of the potentiostat. Increases in pyrrole deposition correlated with a decrease in the peak resonance frequency of the magnetoelastic alloy. This technique provides a novel approach by which one can monitor electrochemical processes.

  16. A Real Time Measuring Method for Complex Impedance in Biomedical Instrumentations

    NASA Astrophysics Data System (ADS)

    Dendo, Isao

    The author proposes a measuring method of complex bioimpedance in real time by using a potentiostat circuit and LabVIEW programming tools. In the system, 4-electrode method is applied on the dc-coupled potentiostat. Complex impedance is calculated from the frequency response function in LabVIEW. The resolutions of the resistive and reactive components are about 0.005% respectively. As a preliminary experiment, the complex impedance on a middle finger at 1kHz is measured with sampling time of 10ms. Pulse waves of resistive components which are synchronizing with ECG are clearly observed and very small reactive components.

  17. Plasma Arc Melting (PAM) and Corrosion Resistance of Pure NiTi Shape Memory Alloys

    NASA Astrophysics Data System (ADS)

    Tuissi, A.; Rondelli, G.; Bassani, P.

    2015-03-01

    Plasma arc melting (PAM) as a suitable non-contaminating melting route for manufacturing high-quality NiTi alloy was successfully examined. The corrosion resistance of PAM Nitinol was evaluated by both potentiodynamic and potentiostatic tests and compared with lower purity NiTi produced by vacuum induction melting (VIM). For the electro-polished surfaces, excellent corrosion resistance of NiTi comparable with the Ti alloys was found with no pitting up to 800 mV versus saturated calomel electrode in simulated body fluid at 37 °C. Potentiostatic results of PAM Nitinol indicate slightly better corrosion resistance than the lower quality VIM alloy.

  18. In situ monitoring of the Li-O2 electrochemical reaction on nanoporous gold using electrochemical AFM.

    PubMed

    Wen, Rui; Byon, Hye Ryung

    2014-03-11

    The lithium-oxygen (Li-O2) electrochemical reaction on nanoporous gold (NPG) is observed using in situ atomic force microscopy (AFM) imaging coupled with potentiostatic measurement. Dense Li2O2 nanoparticles form a film at 2.5 V, which is decomposed at 3.8-4.0 V in an ether-based electrolyte. PMID:24469227

  19. Overview of corrosion, corrosion protection, and stress-corrosion cracking of uranium and uranium alloys

    SciTech Connect

    Koger, J.W.

    1981-12-14

    This paper covers some basic definitions and provides some data. The 51 slides illustrates these definitions, crack initiation and propagation, sources of stress, types of specimens used for SCC, potentiostatic polarization, data for Mulberry and U-Nb alloys, effects of environment, and data for U-0.75 Ti and U-Mo alloys. (DLC)

  20. Toward developing long-life water quality sensors for the ISS using planar REDOX and conductivity sensors

    NASA Technical Reports Server (NTRS)

    Buehler, M. G.; Kuhlman, G. M.; Keymeulen, D.; Myung, N.; Kounaves, S. P.

    2003-01-01

    REDOX and conductivity sensors are metal electrodes that are used to detect ionic species in solution by measuring the electrochemical cell current as the voltage is scanned. This paper describes the construction of the sensors, the potentiostat electronics, the measurement methodology, and applications to water quality measurements.

  1. Affordable Cyclic Voltammetry

    ERIC Educational Resources Information Center

    Stewart, Greg; Kuntzleman, Thomas S.; Amend, John R.; Collins, Michael J.

    2009-01-01

    Cyclic voltammetry is an important component of the undergraduate chemical curriculum. Unfortunately, undergraduate students rarely have the opportunity to conduct experiments in cyclic voltammetry owing to the high cost of potentiostats, which are required to control these experiments. By using MicroLab data acquisition interfaces in conjunction…

  2. AN ADVANCED FLUE GAS MONITOR FOR SO2 - PHASE I

    EPA Science Inventory

    The development of an instrument for continuously monitoring SO2 levels in flue gas is proposed. The SO2 will be detected by means of an electrochemical sensor cell, which operates in a three-electrode potentiostatic mode. The proposed innovation is develop-ment of an advan...

  3. Role of Preparation Method on the Microstructure and Mechanical Properties of PPy/Ni Organic-Inorganic Hybrid Bilayer Coatings on Carbon Steel

    NASA Astrophysics Data System (ADS)

    Torres-Huerta, A. M.; Dominguez-Crespo, M. A.; Alanis-Valdelamar, A.; Onofre-Bustamante, E.; Escudero, M. L.; García-Alonso, M. C.; Lois-Correa, J. A.

    2015-04-01

    The efficacy of the conducting polymers as coating on a metallic substrate is strongly dependent on the manner how they are applied. Polypyrrole (PPy)/Ni organic-inorganic hybrid coatings were electropolymerized on commercial carbon steel (AISI 1018) by combining potentiostatic and potentiodynamic techniques. In first instance, it was analyzed the electrodeposition of PPy using a constant potential regime and cyclic voltammetry techniques evaluating different synthesis parameters such as deposition time, applied potential, and potential cycles, respectively. Thereafter, it was used a potentiostatic method to obtain PPy/Ni bilayer films. The morphological, mechanical, and adhesion properties of these films depend on the synthesis parameters. The results revealed that polypyrrole films formed by both methods provide a globular-type structure, although coatings produced by cyclic voltammetry are denser and slightly thicker than those produced potentiostatically. Ni (oxide/hydroxide) particles are capable of sealing the pores of globular PPy coatings, thus increasing the hardness of the carbon steel (CS)/PPy/Ni system. As a result of the study, we have seen that PPy/Ni bilayer films are more uniform, compact and enhanced the hardness when the PPy is obtained by cyclic voltammetry than that observed for potentiostatic approach. Specifically, when four potential cycles are used to electropolymerized pyrrole, the more convenience properties in the CS/PPy/Ni arrangement are obtained.

  4. Cybernetic Control of an Electrochemical Repertoire.

    ERIC Educational Resources Information Center

    He, Peixin; And Others

    1982-01-01

    Describes major features of a computer-operated, cybernetic potentiostat and the development, design, and operation of the software in ROM. The instrument contains control circuitry and software making it compatible with the static mercury drop electrode produced by EG&G Princeton Applied Research Corporation. Sample results using the instrument…

  5. SEMICONDUCTOR MATERIALS: Morphology dependence of TiO2 nanotube arrays on anodization variables and buffer medium

    NASA Astrophysics Data System (ADS)

    Xin, Wen; Meng, Cao; Jie, Wu; Junchao, Tao; Yan, Sun; Ning, Dai

    2010-06-01

    Vertically oriented TiO2 nanotube arrays were prepared by potentiostatic anodization of Ti foils in HF/acetic acid (HAC) aqueous solution. Anodization variables including anodization electrolyte concentration, anodization voltage, anodization time and buffer medium can be chosen and adjusted to manipulate the nanotube arrays to give the required length and morphology.

  6. Electrochemical behavior of nano and femtosecond laser textured titanium alloy for implant surface modification.

    PubMed

    Jeong, Yong-Hoon; Kim, Won-Gi; Choe, Han-Cheol

    2011-02-01

    In this study, the electrochemical behavior of nano and femtosecond laser textured titanium alloy for implant surface modification has been researched using the potentiostat equipment. Cp-Ti and Ti-6Al-4V alloy, located on X-Y motorized stage, were irradiated using femtosecond laser. The corrosion properties were examined by a potentiodynamic and AC impedance test. PMID:21456241

  7. Electrochemical approach for passivating steel and other metals and for the simultaneous production of a biocide to render water potable

    NASA Technical Reports Server (NTRS)

    1972-01-01

    Potentiostatic polarization curves indicated that the cathodic reactions in deaerated KI-I2 water solutions were due to iodine reduction and hydrogen evolution. In the presence of oxygen an additional reduction wave appeared. Anodic polarization curves revealed that iodine could be produced in the region of potential from +600 to +1000 nv vs. SCE.

  8. Surface pK(sub a) of Self-Assembled Monolayers

    ERIC Educational Resources Information Center

    Hale, Penny S.; Maddox, Leone M.; Shapter, Joe G.

    2005-01-01

    The difference between solution and surface properties such as pK(sub a) is illustrated enabling students to understand the differences between nanoscale and macroscopic systems. Details regarding the usage of electrochemical instrumentation, such as a potentiostat, and of the technique such as cyclic voltammetry are given.

  9. MICROFABRICATED ELECTROCHEMICAL ANALYSIS SYSTEM FOR HEAVY METAL DETECTION. (R825511C047)

    EPA Science Inventory

    A low power, hand-held system has been developed for the measurement of heavy metal ions in aqueous solutions. The system consists of an electrode array sensor, a high performance single chip potentiostat and a microcontroller circuit. The sensor is a microfabricated array of ...

  10. Voltammetry at the Thin-Film Mercury Electrode (TFME).

    ERIC Educational Resources Information Center

    Pomeroy, R. S.; And Others

    1989-01-01

    Reviewed is the use of the Thin-Film Mercury Electrode for anodic stripping voltammetry, simple voltammetry of solution cations and cathodic stripping voltammetry for the determination of an environmentally important molecule, thiourea. The construction of a simple potentiostat and applications for student laboratory courses are included. (CW)

  11. Efficiencies of Bio-electrocatalytic Production of Hydrogen from Lactate Using Shewanella oneidensis MR-1

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Shewanella oneidensis MR-1 was grown in a chemostatic, continuously-fed bioelectrochemical cell under slightly aerated conditions. The start-up phase was controlled potentiostatically (0.4 V vs. SHE). When a stable performance was achieved, the reactor was switched to bio-electrocatalytic producti...

  12. Improvement in the Corrosion Resistance of Austenitic Stainless Steel 316L by Ion Implantation

    NASA Astrophysics Data System (ADS)

    Cai, Xun; Feng, Kai

    In the present work, austenitic stainless steel 316L (SS316L) samples were implanted with Ni and Ni-Cr. A nickel-rich layer about 100 nm in thickness and a Ni-Cr enriched layer about 60 nm thick are formed on the surface of SS316L. The effects of ion implantation on the corrosion performance of SS316L are investigated in a 0.5 M H2SO4 with 2 ppm HF solution at 80°C by open circuit potential (OCP), potentiodynamic and potentiostatic tests. The samples after the potentiostatic test are analyzed by XPS. The results indicate that the composition of the passive film change from a mixture of Fe oxides and Cr oxide to a Cr oxide dominated passive film after the potentiostatic test. The solutions after the potentiostatic test are analyzed by inductively coupled plasma atomic emission spectrometry (ICP-AES). The results reveal that Fe is selectively dissolved in all cases and a proper Ni and Ni-Cr implant fluence can greatly improve the corrosion resistance of SS316L in the simulated polymer electrolyte membrane fuel cells (PEMFCS) environment. They are in agreement with the electrochemical test results that the bare SS316L has the highest dissolution rate in both cathode and anode environments and the Ni and Ni-Cr implantation reduce markedly the dissolution rate. After the potentiostatic test the interfacial contact resistance (ICR) values are also measured. Ni and Ni-Cr are enriched in the passive film formed in the simulated PEMFC cathode environment after ion implantation thereby providing better conductivity than that formed in the anode one. A significant improvement of ICR is achieved for the SS316L implanted with Ni and Ni-Cr as compared to the bare SS316L, which is attributed to the reduction in passive layer thickness caused by Ni and Ni-Cr implantation. The ICR values for implanted specimens increase with increasing dose.

  13. A new electrochemical approach for evaluation of corrosion inhibitors in neutral aqueous solutions

    SciTech Connect

    Jovancicevic, V.; Hartwick, D.

    1997-12-01

    A new comprehensive electrochemical approach to corrosion inhibitor evaluation in neutral aqueous solutions has been developed. It consists of using concurrently three different but complementary electrochemical methods. Linear polarization resistance (LPR), concentration-step potentiostatic (CSP) and constant-concentration potentiostatic (CCP) methods are used to determine the overall corrosion rates, corrosion inhibition mechanism, and stability of the passive oxide film in the presence of corrosion inhibitors. This approach has been used successfully to evaluate corrosion inhibition of three organic inhibitor systems: a phosphonate-based corrosion inhibitor (hydroxyphosphonoacetic acid, HPA), a polymeric corrosion inhibitor (polyacrylic acid, PAA) and a non-phosphorus containing corrosion inhibitor (L-tartaric acid). Short-term CSP/CCP test results for these three inhibitors are in good agreement with long-term weight loss measurements.

  14. Distributed effects of calcium ion contaminant on polymer electrolyte fuel cell performance

    NASA Astrophysics Data System (ADS)

    Uddin, Md Aman; Wang, Xiaofeng; Park, Jaehyung; Pasaogullari, Ugur; Bonville, Leonard

    2015-11-01

    Distributed performance of a polymer electrolyte fuel cell (PEFC) is studied both in galvanostatic and potentiostatic mode during in-situ injection of Ca2+ in the air stream using a segmented cell. In the galvanostatic mode, segments near the inlet are affected first by the contaminant resulting in decreased current density. At the same time, despite the presence of contaminants, current density for the other segments increases in order to maintain constant total current. In the potentiostatic mode, all segments are affected by the contaminants simultaneously and the current density in all segments decreases with time. The performance of the downstream segments is lower than the upstream segments. During both tests, the contaminant is found to precipitate on both the cathode flow field and the cathode GDL surface. As the test progresses, the contaminant penetrates into the GDL and deposits, causing mass transport losses.

  15. Effects of cathodic protection on corrosive wear of 304 stainless steel

    SciTech Connect

    Akonko, Saheed; Li, D.Y.; Ziomek-Moroz, M.

    2005-03-01

    Corrosive wear involves interaction of electrochemical and mechanical processes. The synergism of these two processes often results in significant material loss, compared to those caused by individual processes. Reduction of either corrosion or wear may effectively decrease material loss under certain circumstances. Since cathodic protection can reduce corrosion of metallic materials, it may also diminish corrosive wear if the corrosion process is suppressed. However, under a cathodic potential (potentiostatic condition) or enforced current (galvanosatic condition), properties of a material could be affected and thus its corrosive wear behavior could be different from what is expected. The present research demonstrated that cathodic protection under potentiostatic condition was beneficial under low wearing force but it became ineffective under higher wearing forces or more negative cathodic potentials. Hydrogen embrittlement could be responsible for this change.

  16. Selective dissolution in copper-tin alloys: Formation of corrosion- resistant patina on ancient Chinese bronze mirrors

    SciTech Connect

    Taube, M. |; Davenport, A.J.; King, A.H.; Chase, T. III

    1996-07-01

    Many ancient Chinese bronze mirrors have survived with a patina that leaves the delicate relief surface decorations intact. The microstructure of these ancient mirrors is two-phase and consists of acicular {alpha}-phase (Cu-rich) regions encased in a {delta}-phase (Sn-rich) matrix. At the surface, there is evidence of selective dissolution of the ct phase; the cc-phase regions are replaced pseudomorphically by a mineral product with the {delta} phase remaining metallic. Electrochemical polarization has been used to drive the copper dealloying process in modem, cast bronze. Synchrotron x-ray diffraction was employed to compare the ancient samples with those that were prepared potentiostatically. Poorly crystallized tin oxide (SnO{sub 2}) was found in the {alpha} replacement products of both sample types. The corrosion-resistance of the potentiostatically-treated bronze samples was tested by atmospheric exposure. Comparison with exposed, untreated samples indicated that the treatment was protective.

  17. Template-assisted electrodeposition of indium-antimony nanowires - Comparison of electrochemical methods

    NASA Astrophysics Data System (ADS)

    Hnida, Katarzyna; Mech, Justyna; Sulka, Grzegorz D.

    2013-12-01

    Indium antimonide (InSb) is a III-V compound semiconductor that in a form of nanowires can possess improved thermoelectrical and optical properties compared to the corresponding bulk crystal. Here, we applied three electrodeposition techniques for a fast and inexpensive template-assisted fabrication of InSb nanowires from a sodium citrate-citric acid solution at room temperature. The home-made anodic aluminum oxide (AAO) templates with the pore diameter of 100 nm were used. InSb nanowires were synthesized by potentiostatic, galvanostatic and periodic pulse reverse techniques. The morphology, composition and crystallinity of as-obtained and annealed nanowires were investigated and compared with the literature data. It was found that the potentiostatic and pulse reverse methods gave crystalline nanowires. On the other hand, the constant current density deposition results in a partially amorphous nanowire material.

  18. Design and Fabrication of Complementary Metal-Oxide-Semiconductor Sensor Chip for Electrochemical Measurement

    NASA Astrophysics Data System (ADS)

    Yamazaki, Tomoyuki; Ikeda, Takaaki; Kano, Yoshiko; Takao, Hidekuni; Ishida, Makoto; Sawada, Kazuaki

    2010-04-01

    An electrochemical sensor has been developed on a single chip in which potentiostat and sensor electrodes are integrated. Sensor chips were fabricated using 5.0 µm complementary metal-oxide-semiconductor (CMOS) technology. All processes including the CMOS process, postprocessing for fabricating sensor electrodes and passivation layers, and packaging were performed at Toyohashi University of Technology. The integration makes it possible to measure electrochemical signals without having to use a bulky external electrochemical system. The potential between the working electrode and the reference electrode was controlled using an on-chip potentiostat composed of CMOS transistors. The chip characteristics were verified by electrochemical measurement, namely, by cyclic voltammetry. Potassium ferricyanide solution was measured to obtain results that fit well to the theoretical formula. A clear proportional relationship between peak height and the concentration of the sample solution was obtained using the proposed sensor chip, and the dynamic range obtained was 0.10 to 8.0 mM.

  19. Design and Fabrication of Complementary Metal-Oxide-Semiconductor Sensor Chip for Electrochemical Measurement

    NASA Astrophysics Data System (ADS)

    Tomoyuki Yamazaki,; Takaaki Ikeda,; Yoshiko Kano,; Hidekuni Takao,; Makoto Ishida,; Kazuaki Sawada,

    2010-04-01

    An electrochemical sensor has been developed on a single chip in which potentiostat and sensor electrodes are integrated. Sensor chips were fabricated using 5.0 μm complementary metal-oxide-semiconductor (CMOS) technology. All processes including the CMOS process, postprocessing for fabricating sensor electrodes and passivation layers, and packaging were performed at Toyohashi University of Technology. The integration makes it possible to measure electrochemical signals without having to use a bulky external electrochemical system. The potential between the working electrode and the reference electrode was controlled using an on-chip potentiostat composed of CMOS transistors. The chip characteristics were verified by electrochemical measurement, namely, by cyclic voltammetry. Potassium ferricyanide solution was measured to obtain results that fit well to the theoretical formula. A clear proportional relationship between peak height and the concentration of the sample solution was obtained using the proposed sensor chip, and the dynamic range obtained was 0.10 to 8.0 mM.

  20. Effects of pulse voltage on the formation of nanoporous Ti oxides by dealloying amorphous TiCu alloy

    NASA Astrophysics Data System (ADS)

    Zhu, Shengli; Pi, Lele; Xie, Guoqiang; Cui, Zhenduo; Yang, Xianjin; Inoue, Akihisa

    2013-03-01

    In present study, we prepared nanoporous Ti oxides by potentiostat and pulse dealloying TiCu amorphous alloy in HNO3 solution. The influence of applied voltage on the morphology was investigated by SEM. The mechanism of dealloying was also discussed. A multilayer nanoporous structure was fabricated using pulse dealloying. The ideal nanoporous structure with mean pore diameter of about 50-100 nm and mean pore wall thickness of about 50 nm was obtained using pulse dealloying with initial voltage of 1.0 V and pulse size of 0.4 V. The static currents for pulse dealloying are higher than those for potentiostat dealloying under the same initial potentials. The nanoporous surface is mainly composed of TiO, Ti2O3 and TiO2.

  1. Teorell instability in concentration polarization

    NASA Astrophysics Data System (ADS)

    Abu-Rjal, Ramadan; Prigozhin, Leonid; Rubinstein, Isaak; Zaltzman, Boris

    2015-08-01

    We investigate the development of electro-osmotic (Teorell) oscillations at a weakly charged microporous membrane without a preimposed transmembrane electrolyte concentration drop. This drop, necessary for the occurrence of oscillations, develops spontaneously as a result of concentration polarization in the solution layers adjacent to the membrane. A three-layer model comprising a membrane flanked by two diffusion layers is proposed and analyzed for galvano- and potentiostatic regimes of operation.

  2. On-line corrosion monitoring with electrochemical impedance spectroscopy

    SciTech Connect

    Roberge, P.R. . Dept. of Chemistry and Chemical Engineering); Sastri, V.S. )

    1994-10-01

    Electrochemical impedance spectroscopy (EIS) has been found to be a rapid and accurate technique for measuring corrosion rates in the most difficult situations and for yielding information concerning the occurrence of localized corrosion. When used in the absence of potentiostatic control, the technique carries less instrumental overhead, and the danger of damaging the probe by accidental polarization is reduced. Results from two field tests were presented to illustrate the advantages of using EIS for on-line monitoring of general and localized corrosion.

  3. Highly Methanol Tolerant Cathode Based on PtAg for Use in Microfluidic Fuel Cell

    NASA Astrophysics Data System (ADS)

    Abrego-Martínez, J. C.; Mendoza-Huizar, L. H.; Ledesma-Garcia, J.; Arriaga, L. G.; Cuevas-Muñiz, F. M.

    2015-12-01

    In the present work, a methanol tolerant cathode catalyst was developed through the electrodeposition of bimetallic nanoparticles PtAg on a glassy carbon electrode using potentiostatic and voltammetric techniques. The resulting particles were characterized by Scanning Electron Microscopy (SEM) and electrochemical techniques. According to the SEM study the synthetized nanoparticles have semi-spherical shape and their average diameter is 100 nm. This material shows catalytic activity to the oxygen reduction reaction with high tolerance to methanol.

  4. Demonstration of lithographic patterning in measurements of general and localized corrosion on alloy 22

    SciTech Connect

    Bedrossian, P J; Farmer, J C

    1999-07-01

    We have demonstrated a new technique capable of detecting generalized corrosion of metallographically-polished materials with nanometer-scale precision. After exposing a lithographically-patterned coupon of Alloy 22 to an electrolyte in a potentiostatically-controlled cell for twenty-four hours, we detected the loss of up to 130nm of metal. In addition, ''wormholes'' were detected at certain points of intersection of three grain boundaries.

  5. Experimental Setup

    NASA Astrophysics Data System (ADS)

    Stojek, Zbigniew

    To run a successful electrochemical experiment it is essential that the experimental setup is electrically correct and appropriate for the experiment planned. There are several points that should be carefully considered before the experiments are started. They include proper choice of the working, reference and auxiliary electrodes, proper selection of the solvent and supporting electrolyte, proper selection of the electroanalytical technique and its parameters, proper wiring of the electrochemical circuit and, finally, proper setting of the parameters of the potentiostat/voltammograph used.

  6. Electrochemically controlled proton-transfer-catalyzed reactions at liquid-liquid interfaces: nucleophilic substitution on ferrocene methanol.

    PubMed

    Peljo, Pekka; Qiao, Liang; Murtomäki, Lasse; Johans, Christoffer; Girault, Hubert H; Kontturi, Kyösti

    2013-02-01

    The generation of α-ferrocenyl carbocations from ferrocenyl alcohols for S(N)1 substitution at the water-organic solvent interface is initiated by the transfer of protons into the organic phase. The proton flux, and hence the reaction rate, can be controlled by addition of a suitable "phase-transfer catalyst" anion or by external polarization with a potentiostat, providing a new method for the synthesis of ferrocene derivatives. PMID:23225302

  7. Controlled Zn-mediated grafting of thin layers of bipodal diazonium salt on gold and carbon substrates.

    PubMed

    Torréns, Mabel; Ortiz, Mayreli; Turner, Anthony P F; Beni, Valerio; O'Sullivan, Ciara K

    2015-01-01

    A controlled, rapid, and potentiostat-free method has been developed for grafting the diazonium salt (3,5-bis(4-diazophenoxy)benzoic acid tetrafluoroborate (DCOOH)) on gold and carbon substrates, based on a Zn-mediated chemical dediazonation. The highly stable thin layer organic platforms obtained were characterized by cyclic voltammetry, AFM, impedance, XP, and Raman spectroscopies. A dediazonation mechanism based on radical formation is proposed. Finally, DCOOH was proved as a linker to an aminated electroactive probe. PMID:25377261

  8. Studying localized corrosion using liquid cell transmission electron microscopy

    SciTech Connect

    Chee, See Wee; Pratt, Sarah H.; Hattar, Khalid; Duquette, David; Ross, Frances M.; Hull, Robert

    2014-11-07

    Using liquid cell transmission electron microscopy (LCTEM), localized corrosion of Cu and Al thin films immersed in aqueous NaCl solutions was studied. We demonstrate that potentiostatic control can be used to initiate pitting and that local compositional changes, due to focused ion beam implantation of Au+ ions, can modify the corrosion susceptibility of Al films. Likewise, a discussion on strategies to control the onset of pitting is also presented.

  9. Studying localized corrosion using liquid cell transmission electron microscopy

    DOE PAGESBeta

    Chee, See Wee; Pratt, Sarah H.; Hattar, Khalid; Duquette, David; Ross, Frances M.; Hull, Robert

    2014-11-07

    Using liquid cell transmission electron microscopy (LCTEM), localized corrosion of Cu and Al thin films immersed in aqueous NaCl solutions was studied. We demonstrate that potentiostatic control can be used to initiate pitting and that local compositional changes, due to focused ion beam implantation of Au+ ions, can modify the corrosion susceptibility of Al films. Likewise, a discussion on strategies to control the onset of pitting is also presented.

  10. A Scanning Auger Microprobe analysis of corrosion products associated with sulfate reducing bacteria

    SciTech Connect

    Sadowski, R.A.; Chen, G.; Clayton, C.R.; Kearns, J.R.; Gillow, J.B.; Francis, A.J.

    1995-03-01

    A Scanning Auger Microprobe analysis was performed on the corrosion products of an austenitic AISI type 304 SS after a potentiostatic polarization of one volt for ten minutes in a modified Postgate`s C media containing sulfate reducing bacteria. The corrosion products were characterized and mapped in local regions where pitting was observed. A critical evaluation of the applicability of this technique for the examination of microbially influenced corrosion (MIC) is presented.

  11. A Scanning Auger Microprobe analysis of corrosion products associated with sulfate reducing bacteria

    SciTech Connect

    Sadowski, R.A.; Chen, G.; Clayton, C.R.; Kearns, J.R.; Gillow, J.B.; Francis, A.J.

    1995-10-01

    A Scanning Auger Microprobe analysis was performed on the corrosion products of an austenitic AISI type 304 ss after a potentiostatic polarization of one volt for ten minutes in a modified Postgate`s C media containing sulfate reducing bacteria. The corrosion products were characterized and mapped in local regions where pitting was observed. A critical evaluation of the applicability of this technique for the examination of Microbially influenced corrosion (MIC) is presented.

  12. A Low-Cost Smartphone-Based Electrochemical Biosensor for Point-of-Care Diagnostics

    PubMed Central

    Sun, Alexander; Wambach, Travis; Venkatesh, A. G.; Hall, Drew A.

    2015-01-01

    This paper describes the development of a smartphone-based electrochemical biosensor module. The module contains a low power potentiostat that interfaces and harvests power from a smartphone through the phone’s audio jack. A prototype with two different potentiostat designs was constructed and used to conduct proof of concept cyclic voltammetry experiments with potassium ferro-/ferricyanide (K4[Fe(CN)6] / K3[Fe(CN)6]) in a side-by-side comparison with a laboratory grade instrument. Results show that the module functions within the available power budget and that the recovered voltammogram data matches well with the data from an expensive bench top tool. Excluding the loses from supply rectification and regulation, the module consumes either 5.7 mW or 4.3 mW peak power, depending on which of the two discussed potentiostat designs is used. At single quantity pricing, the hardware for the prototype device costs less than $30. PMID:26097899

  13. A CMOS Amperometric System for Multi-Neurotransmitter Detection.

    PubMed

    Massicotte, Genevieve; Carrara, Sandro; Di Micheli, Giovanni; Sawan, Mohamad

    2016-06-01

    In vivo multi-target and selective concentration monitoring of neurotransmitters can help to unravel the brain chemical complex signaling interplay. This paper presents a dedicated integrated potentiostat transducer circuit and its selective electrode interface. A custom 2-electrode time-based potentiostat circuit was fabricated with 0.13 μm CMOS technology and provides a wide dynamic input current range of 20 pA to 600 nA with 56 μ W, for a minimum sampling frequency of 1.25 kHz. A multi-working electrode chip is functionalized with carbon nanotubes (CNT)-based chemical coatings that offer high sensitivity and selectivity towards electroactive dopamine and non-electroactive glutamate. The prototype was experimentally tested with different concentrations levels of both neurotransmitter types, and results were similar to measurements with a commercially available potentiostat. This paper validates the functionality of the proposed biosensor, and demonstrates its potential for the selective detection of a large number of neurochemicals. PMID:26761882

  14. Electrochemical sensing of nuclear matrix protein 22 in urine with molecularly imprinted poly(ethylene-co-vinyl alcohol) coated zinc oxide nanorod arrays for clinical studies of bladder cancer diagnosis.

    PubMed

    Lee, Mei-Hwa; Thomas, James L; Chang, Yu-Chia; Tsai, Yuh-Shyan; Liu, Bin-Da; Lin, Hung-Yin

    2016-05-15

    In 1996 and 2000, the US Food and Drug Administration (FDA) approved the use of Nuclear matrix protein 22 (NMP22) as a monitoring tool for predicting the recurrence/clearing of bladder cancer, and for screening undiagnosed individuals who have symptoms of, or are at risk for, that disease. The fabrication of electrodes for sensing NMP22 and their integration with a portable potentiostat in a homecare system may have great value. This work describes a sensing element comprised of molecularly imprinted polymers (MIPs) for the specific recognition of NMP22 target molecules. Zinc oxide (ZnO) nanorods (214±45nm in diameter and 1.08±0.11μm long) were hydrothermally grown on the sensing electrodes to increase the surface area to be coated with MIPs. A portable potentiostat was assembled and a data acquisition (DAQ) card and the Labview program were utilized to monitor electrochemical reaction to sense NMP22 in urine samples. Finally, in phase 0 clinical trials, measurements were made of samples from a few patients with bladder cancer using the NMP22 MIP-coated ZnO nanorods electrodes that were integrated into a portable potentiostat, revealing NMP 22 concentrations in the range 128±19 to 588±53ng/mL. PMID:26774095

  15. Effect of chemical etching and aging in boiling water on the corrosion resistance of Nitinol wires with black oxide resulting from manufacturing process.

    PubMed

    Shabalovskaya, S; Rondelli, G; Anderegg, J; Simpson, B; Budko, S

    2003-07-15

    The effect of chemical etching in a HF/HNO(3) acid solution and aging in boiling water on the corrosion resistance of Nitinol wires with black oxide has been evaluated with the use of potentiodynamic, modified potentiostatic ASTM F746, and scratch tests. Scanning-electron microscopy, elemental XPS, and Auger analysis were employed to characterize surface alterations induced by surface treatment and corrosion testing. The effect of aging in boiling water on the temperatures of martensitic transformations and shape recovery was evaluated by means of measuring the wire electroresistance. After corrosion tests, as-received wires revealed uniformly cracked surfaces reminiscent of the stress-corrosion-cracking phenomenon. These wires exhibited negative breakdown potentials in potentiostatic tests and variable breakdown potentials in potentiodynamic tests (- 100 mV to + 400 mV versus SCE). Wires with treated surfaces did not reveal cracking or other traces of corrosion attacks in potentiodynamic tests up to + 900-1400-mV potentials and no pitting after stimulation at + 800 mV in potentiostatic tests. They exhibited corrosion behavior satisfactory for medical applications. Significant improvement of corrosion parameters was observed on the reverse scans in potentiodynamic tests after exposure of treated wires to potentials > 1000 mV. In scratch tests, the prepared surfaces repassivated only at low potentials, comparable to that of stainless steel. Tremendous improvement of the corrosion behavior of treated Nitinol wires is associated with the removal of defect surface material and the growth of stable TiO(2) oxide. The role of precipitates in the corrosion resistance of Nitinol-scratch repassivation capacity in particular-is emphasized in the discussion. PMID:12808592

  16. Convection of tin in a Bridgman system. II - An electrochemical method for detecting flow regimes

    NASA Astrophysics Data System (ADS)

    Sears, B.; Fripp, A. L.; Debnam, W. J., Jr.; Woodell, G. A.; Anderson, T. J.; Narayanan, R.

    1992-12-01

    An ampoule was designed in order to obtain local flow behavior of the flow fields for convection of tin in a vertical Bridgman configuration. Multiple electrochemical cells were located along the periphery of the ampoule. Oxygen was titrated into the ampoule at one of the cell locations using a potentiostat and the concentration of oxygen was monitored at the other cell locations by operating the cells in a galvanic mode. Onset of oscillations were detected by means of thermocouples. We conclude that the flows are generally three dimensional for an aspect ratio of 5. Results on oscillations concurred with those of earlier workers. Suggestions for improved designs were made.

  17. Studies of passive film breakdown by detection and analysis of electrochemical noise

    NASA Astrophysics Data System (ADS)

    Bertocci, U.; Kruger, J.

    1980-12-01

    Random fluctuations in the passive current of electrodes under potentiostatic conditions have been measured on aluminum in boric acid: borate solution and on a Fe-Cr-Ni alloy, both in the amorphous and in the crystalline state, in sulfuric acid. The onset of pitting can be detected by thc large increase in current noise. The noise level is different in the amorphous and crystalline Fe-Cr-Ni alloy, indicating that the breakdown of the passive film differs in the two conditions. Thc experimental aspects involved in carrying out meaningful noise measurements in electrochemical systems are also discussed.

  18. Patterned electrochemical deposition of copper using an electron beam

    SciTech Connect

    Heijer, Mark den; Shao, Ingrid; Reuter, Mark C.; Ross, Frances M.; Radisic, Alex

    2014-02-01

    We describe a technique for patterning clusters of metal using electrochemical deposition. By operating an electrochemical cell in the transmission electron microscope, we deposit Cu on Au under potentiostatic conditions. For acidified copper sulphate electrolytes, nucleation occurs uniformly over the electrode. However, when chloride ions are added there is a range of applied potentials over which nucleation occurs only in areas irradiated by the electron beam. By scanning the beam we control nucleation to form patterns of deposited copper. We discuss the mechanism for this effect in terms of electron beam-induced reactions with copper chloride, and consider possible applications.

  19. Separation of metal ions from aqueous solutions

    DOEpatents

    Almon, Amy C.

    1994-01-01

    A process and apparatus for quantitatively and selectively separating metal ions from mixtures thereof in aqueous solution. The apparatus includes, in combination, a horizontal electrochemical flow cell containing flow bulk electrolyte solution and an aqueous, metal ion-containing solution, the cell containing a metal mesh working electrode, a counter electrode positioned downstream from the working electrode, an independent variable power supply/potentiostat positioned outside of the flow cell and connected to the electrodes, and optionally a detector such as a chromatographic detector, positioned outside the flow cell. This apparatus and its operation has significant application where trace amounts of metal ions are to be separated.

  20. Over 95% of large-scale length uniformity in template-assisted electrodeposited nanowires by subzero-temperature electrodeposition

    PubMed Central

    2011-01-01

    In this work, we report highly uniform growth of template-assisted electrodeposited copper nanowires on a large area by lowering the deposition temperature down to subzero centigrade. Even with highly disordered commercial porous anodic aluminum oxide template and conventional potentiostatic electrodeposition, length uniformity over 95% can be achieved when the deposition temperature is lowered down to -2.4°C. Decreased diffusion coefficient and ion concentration gradient due to the lowered deposition temperature effectively reduces ion diffusion rate, thereby favors uniform nanowire growth. Moreover, by varying the deposition temperature, we show that also the pore nucleation and the crystallinity can be controlled. PMID:21781335

  1. Morphology, structure, and magnetism of FeCo thin films electrodeposited on hydrogen-terminated Si(111) surfaces.

    PubMed

    Zarpellon, J; Jurca, H F; Mattoso, N; Klein, J J; Schreiner, W H; Ardisson, J D; Macedo, W A A; Mosca, D H

    2007-12-15

    In this work we describe the fabrication of FeCo alloy (less than 10 at% Co) thin films from aqueous ammonium sulfate solutions onto n-type Si(111) substrates using potentiostatic electrodeposition at room temperature. The incorporation of Co into the deposits tends to inhibit Fe silicide formation and to protect deposits against oxidation under air exposure. As the incorporation of Co was progressively increased, the sizes of nuclei consisting of FeCo alloy increased, leading to films with a highly oriented body-centered cubic structure with crystalline texture, where (110) planes remain preferentially oriented parallel to the film surface. PMID:17900605

  2. Mechanism of the discharging of lanthanum and yttrium ions on a solid cathode in molten chlorides

    SciTech Connect

    Shkol'nikov, S.N.; Tolypin, E.S.; Zatitskii, B.E.

    1982-07-20

    This work attempted to investigate the mechanism of the discharging of La/sup 3 +/ and Y/sup 3 +/ ions on a solid cathode in molten chlorides and to calculate the kinetic parameters of these processes by the main potentiostatic method. The theory of the method was outlined in rather great detail in the literature. Results indicated that on the whole, the kinetic rate constants of the electrode processes are rather large, which permits these reactions to be considered as quasi-reversible.

  3. Behavior of alloys of the PtPd intermetallic compound with Hf and Zr in the electrosynthesis of peroxo salts

    SciTech Connect

    Toroptseva, N.T.; Vaseva, A.Yu.

    1988-08-10

    The objective of this study was to investigate the behavior of anodes made of alloys of the PtPd intermetallic compound with Hf and Zr in the synthesis of potassium peroxodicarbonates and peroxoborates. The investigations were based on polarization measurements in different regimes on stationary and rotating electrodes, the determination of the current yield of active oxygen in galvano- and potentiostatic syntheses, and the study of the kinetics of catalytic decomposition of peroxide solutions in the presence of the electrode in the range 289-308 K.

  4. Recording and analysis of AC impedance data for corrosion studies II. Experimental approach and results

    SciTech Connect

    Mansfeld, F.; Kendig, M.W.; Tsai, S.

    1982-11-01

    Experimental approaches for recording ac impedance data are discussed in this paper. Considerations of the high frequency performance of potentiostats and reference electrodes are given and experimental results are presented. Additional methods for analysis of experimental impedance data are discussed, with emphasis on the CIRFIT computer program. +BTA and Al 2024/3.5% NaCl are discussed in detail. Pitting of the Al alloy in neutral NaCl leads to a second time constant at low frequencies. Results for iron and Al 2024 in tapwater show that the low conductivity does not present particular problems with the recording of ac impedance data.

  5. Electrochemical techniques for the characterisation of expander materials

    NASA Astrophysics Data System (ADS)

    Francia, Carlotta; Maja, Mario; Spinelli, Paolo; Saez, Francisco; Martinez, Bruno; Marin, Dolores

    Characterisation of expander materials has been obtained by comparing the results of three different electrochemical techniques: cyclic voltammetry, potentiostatic transients and electrochemical impedance. It is shown that the evaluation of the expanders' performance carried out on the basis of the results of such techniques takes into account different important actions of the organic additives such as adsorption on lead and kinetics of electrochemical reactions. Seventeen different organic substances have been tested including both commercial materials used in the lead-acid battery industry, and other materials presenting physico-chemical similarities to known expanders.

  6. Electrochemical apparatus for automatic measurement of carrier-concentration distribution in semiconductors

    SciTech Connect

    Belova, N.A.; Galchenkov, L.A.; Skvortsova, N.E.

    1986-06-01

    This paper describes apparatus for measuring the carrier-concentration depth (from 1 to 30-50 um) distribution of semiconductors in the concentration range of 10/sup 14/-10/sup 19/ cm/sup -3/. The measurement errors for concentration and depth are 10% and 5%. Measurements can be made in AgAs, InP, Si, and, with proper selection of the electrolyte, other semiconductors. Measurements are made automatically and the results are recorded with a plotter. Schematic diagrams are presented of the main units of the apparatus which include the capacitance meter, synchronous detector, potentiostat, automatic unit, and various circuits.

  7. Dynamics and Topography of QUASI-2D Needle-Like Silver Electrochemical Deposits Under a Quasi-Steady Regime

    NASA Astrophysics Data System (ADS)

    Pasquale, M. A.; Vicente, J. L.; Arvia, A. J.

    The electrochemical formation of single silver needles from aqueous silver sulfate was studied under both potentiostatic and galvanostatic conditions utilizing different quasi-2D cells. Under potentiostatic conditions, four (I-IV) stages of growth were distinguished. Stage III involved single needle growth under a quasi-steady-state (q-ss) regime in which, at the millimeter scale, the tip profile remained almost unchanged. Fast growing needles exhibited a truncated quasi-conical tip, and slow growing ones approached prolate hemispheroids. At stage III, the almost constant q-ss silver deposition rate was evaluated from the tip front displacement (dLz/dt) perpendicularly to the tangential plane of the tip. For the cathode to anode potential difference in the range -1.00 ? Ec-a ? -0.22 V, values of (dLz/dt) in the range 0.08-2.0 ?m s-1 were obtained. At the needle stem, the q-ss radial silver deposition rate (dLx/dt) was about two orders of magnitude lower than (dLz/dt). The transition from stage III to IV was characterized by tip thickening, i.e. a change in the tip q-conical profile to that of a prolate hemispheroid, and eventual tip splitting. Scanning electron micrographs at the micrometer scale of single silver needle tips from potentiostatic runs showed either a defined crystallography or an irregular topography covered by a large number of tiny crystals. In contrast, stems were always faceted. This difference indicated that surface relaxation processes following silver ion mass transport and discharge played a relevant role in the needle growth mode. At stage III, the growth regime is described utilizing a dual diffusion (D) and migration (M) model consisting of a DM direct contribution that becomes dominant at the needle stem, and a space charge (SC)-assisted DM contribution that operates at the tip apex. This explanation is consistent with the local cathodic current density values, the concentration ratio of silver clusters at the stem and tip apex surface, and the distinct kinetic behavior of needles produced from potentiostatic and galvanostatic runs. The complex link between mass transport phenomena of silver ions from the binary solution side, the silver ion discharge at the interface and the surface relaxation of silver adatoms and clusters at the metal lattice shed new light on the aspects of single silver needle formation.

  8. The effect of potential upon the high-temperature fatigue crack growth response of low-alloy steels. Part 1: Crack growth results

    SciTech Connect

    James, L.A.; Moshier, W.C.

    1997-04-01

    Corrosion-fatigue crack propagation experiments were conducted on several low-alloy steels in elevated temperature aqueous environments, and experimental parameters included temperature, sulfur content of the steel, applied potential level, and dissolved hydrogen (and in one case, dissolved oxygen) concentration in the water. Specimen potentials were controlled potentiostatically, and the observation (or non-observation) of accelerated fatigue crack growth rates was a complex function of the above parameters. Electrochemical results and the postulated explanation for the complex behavior are given in Part II.

  9. Electrodeposition of a tellurium-iodine compound

    SciTech Connect

    Bigelis, V.M.

    1988-01-01

    Forming more stable tellurium in iodide solution was investigated. Solutions with a large excess of iodide ions were prepared and radiotracers measured the current yields of tellurium. A platinum sheet was used as cathode, a tellurium rod was the anode, and a saturated silver-silver chloride electrode was the reference electrode. Electrodeposition and polarization measurements were conducted by a potentiostat. Polarization curves were obtained. Iodine 125 and tellurium 123m were used in the radiochemical analysis of the deposition yield and rate. Radioactivity measurements were made with a Ge(Li) detector.

  10. Convection of tin in a Bridgman system. II - An electrochemical method for detecting flow regimes

    NASA Technical Reports Server (NTRS)

    Sears, B.; Fripp, A. L.; Debnam, W. J., Jr.; Woodell, G. A.; Anderson, T. J.; Narayanan, R.

    1992-01-01

    An ampoule was designed in order to obtain local flow behavior of the flow fields for convection of tin in a vertical Bridgman configuration. Multiple electrochemical cells were located along the periphery of the ampoule. Oxygen was titrated into the ampoule at one of the cell locations using a potentiostat and the concentration of oxygen was monitored at the other cell locations by operating the cells in a galvanic mode. Onset of oscillations were detected by means of thermocouples. We conclude that the flows are generally three dimensional for an aspect ratio of 5. Results on oscillations concurred with those of earlier workers. Suggestions for improved designs were made.

  11. Current-Voltage Characteristics of Electrolyte-Gated Graphene Field-Effect Transistors

    NASA Astrophysics Data System (ADS)

    Meric, Inanc; Sorgenfrei, Sebastian; Han, Melinda; Oezyilmaz, Barbaros; Kim, Philip; Shepard, Kenneth

    2008-03-01

    We investigate the current-voltage characteristics of graphene field-effect transistors (FET) with ionic-solution gating. Single-layer graphene FETs are fabricated with different device dimensions and electrolytically gated with a potentiostat in which a Pt counter electrode and an Ag/AgCl reference electrode in a feedback configuration hold the solution at a desired potential. This setup enables the gating of graphene with high efficiency due to the short Debye length and high dielectric constant in ionic solutions, leading to enhanced measured transconductances. Electrolytic gating has direct applicability to field-effect sensor applications of graphene devices.

  12. Electrochemical Reactions During Ru Chemical Mechanical Planarization and Safety Considerations

    NASA Astrophysics Data System (ADS)

    Shima, Shohei; Wada, Yutaka; Tokushige, Katsuhiko; Fukunaga, Akira; Tsujimura, Manabu

    2011-05-01

    We analyzed electrochemical reactions during ruthenium (Ru) chemical mechanical planarization (CMP) using a potentiostat and a quartz crystal microbalance, and considered the potential safety issues. We evaluated the valence number derived from Faraday's law using the dissolution mass change of Ru and total coulomb consumption in the electrochemical reactions for Ru in acidic solution and slurry. The valence numbers of dissolved Ru ions were distributed in the range of 2 to 3.5. As toxic ruthenium tetroxide (RuO4) has a valence number of 8, we were able to conclude that no toxic RuO4 was produced in the actual Ru CMP.

  13. Microfluidic platform for neurotransmitter sensing based on cyclic voltammetry and dielectrophoresis for in vitro experiments.

    PubMed

    Mathault, Jessy; Zamprogno, Pauline; Greener, Jesse; Miled, Amine

    2015-08-01

    This paper presents a new microfluidic platform that can simultaneously measure and locally modulate neurotransmitter concentration in a neuron network. This work focuses on the development of a first prototype including a potentiostat and electrode functionalization to detect several neurotransmitter's simultaneously. We tested dopamine as proof of concept to validate functionality. The system is based on 320 bidirectional electrode array for dielectrophoretic manipulation and cyclic voltammetry. Each electrode is connected to a mechanical multiplexer in order to reduce noise interference and fully isolate the electrode. The multiplexing rate is 476 kHz and each electrode can drive a signal with an amplitude of 60 V pp for dielectrophoretic manipulation. PMID:26736720

  14. Extensive study of shape and surface structure formation in the mercury beating heart system.

    PubMed

    Ramírez-Álvarez, E; Ocampo-Espindola, J L; Montoya, Fernando; Yousif, F; Vázquez, F; Rivera, M

    2014-11-13

    A phenomenological study of the mercury beating heart system in a three electrode electrochemical cell configuration forced with a harmonic perturbation is presented. The system is controlled via a potentiostat, where the mercury drop is electrically connected to a platinum wire and acts as the working electrode. This configuration exhibits geometrical shapes and complex surface structures when a harmonic signal is superimposed to the working electrode potential. This study involves a wide range of frequencies and amplitudes of the forcing signal. Differents levels of structure complexity are observed as a function of the parameters of the applied perturbation. At certain amplitudes and frequencies, rotational behavior is also observed. PMID:25343208

  15. Electrical/thermoelectric characterization of electrodeposited Bi x Sb2- x Te3 thin films

    NASA Astrophysics Data System (ADS)

    Yoo, In-Joon; Lim, Dong Chan; Myung, Nosang V.; Jeong, Young-Keun; Kim, Yang Do; Lee, Kyu Hwan; Lim, Jae-Hong

    2013-09-01

    Bi x Sb2- x Te3 films were electrodeposited potentiostatically from acidic nitric baths at room temperature by controlling the electrodeposition parameters (i.e., the applied potential). Nearly stoichiometric Bi x Sb2- x Te3 thin films were obtained at applied potentials between -0.10 and -0.15 V versus the saturated calomel electrode (SCE). The electrical and thermoelectric properties of the as-deposited films were degraded at more negative deposition potentials; this might be attributed to the greater defect density formed. The post-annealing process in the reducing environment improved the electrical and thermoelectric properties, possibly because of a decrease in antistructure defects.

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

    NASA Astrophysics Data System (ADS)

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

    2016-03-01

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

  17. Effects of magnetic fields from underwater electrical cutting on in vitro corrosion of dental amalgam

    SciTech Connect

    Ortendahl, T.W.; Hoegstedt, P.O.; Odelius, H.; Noren, J.G.

    1988-11-01

    Metallic taste has been reported from divers working with underwater electric welding and cutting. An in vitro model was designed to simulate the intraoral situation of the divers with respect to the magnetic field. Potentiostatic analyses were performed on amalgam samples exposed to AC and DC magnetic fields. Morphologic changes were analyzed using differential interference light microscopy and scanning electron microscopy. Chemical changes on the surface of the amalgam samples were analyzed with secondary ion mass spectrometry. Results demonstrated that dental amalgams exposed to a specific AC magnetic field underwent morphologic and chemical changes in the superficial amalgam layers.

  18. Reduction of Plutonium in Acidic Solutions by Mesoporous Carbons

    DOE PAGESBeta

    Parsons-Moss, Tashi; Jones, Stephen; Wang, Jinxiu; Wu, Zhangxiong; Uribe, Eva; Zhao, Dongyuan; Nitsche, Heino

    2015-12-19

    Batch contact experiments with several porous carbon materials showed that carbon solids spontaneously reduce the oxidation state of plutonium in 1-1.5 M acid solutions, without significant adsorption. The final oxidation state and rate of Pu reduction varies with the solution matrix, and also depends on the surface chemistry and surface area of the carbon. It was demonstrated that acidic Pu(VI) solutions can be reduced to Pu(III) by passing through a column of porous carbon particles, offering an easy alternative to electrolysis with a potentiostat.

  19. The ethanol electrooxidation at Pt layers deposited on polycrystalline Au.

    PubMed

    Prieto, Mauricio J; Rodrigues Filho, Ubirajara P; Landers, Richard; Tremiliosi-Filho, Germano

    2012-01-14

    The ethanol electro-oxidation reaction was evaluated using a polycrystalline Au substrate modified with two different amounts of Pt using the galvanic exchange methodology. FTIR results suggest that Pt deposits have a greater ability to break the C-C bond present in the ethanol molecule. However, under potentiostatic conditions both modified Au surfaces undergo faster deactivation in comparison with polycrystalline platinum as indicated by the chronoamperometric results. XPS results indicate the presence of two phases depending on the Pt content. These are: (i) Pt-Au alloy and (ii) segregated Pt. The structural and electronic properties of these phases were related to the differences observed in the catalytic activity. PMID:22116267

  20. A model for nanolaminated growth patterns in Zn and Zn-Co electrodeposits

    SciTech Connect

    Yan, H.; Downes, J.; Boden, P.J.; Harris, S.J.

    1996-05-01

    A hydroxide oscillation model has been proposed to account for the observed nanolaminated structure in electrodeposited Zn and Zn-Co alloys produced under potentiostatic control. At a critical cathode potential the Zn deposition proceeds in a cyclically changing environment arising from the regular formation and decay of a zinc hydroxide layer near the cathode surface, which produces Zn-ZnO laminations in the deposits. Co was found to enrich at the Zn-ZnO interface. Such a model is supported by evidence obtained from electrochemical measurements and transmission electron microscopy observations, and this has given some insight into the anomalous behavior of Zn-Co deposition.

  1. Influence of dissolved hydrogen on aluminum-lithium alloy fracture behavior

    NASA Technical Reports Server (NTRS)

    Rivet, F. C.; Swanson, R. E.

    1989-01-01

    The objective of this work is to study the effects of dissolved hydrogen on the mechanical properties of 2090 and 2219 alloys. Prior to mechanical testing, potentiostatic and potentiodynamic tests were performed using NaCl/HCl solutions varying in pH from 1.5 to 7.5 (3.5 pct NaCl in deionized water). After analysis of the potentiodynamic curve for each solution, several potentiostatic experiments were conducted for various times (from 10 minutes to several hours) with a cathodic overpotential of 300 mV. These experiments were performed to select charging conditions. It is shown that the fracture of L-S and T-S orientations proceeds via slipping of layers in the S-T direction. The T-S and L-S orientations fractured with substantially higher propagation energy that the L-T and T-L orientations, due in large part to the extensive delamination propagation of the fracture.

  2. Growth and etch rate study of low temperature anodic silicon dioxide thin films.

    PubMed

    Ashok, Akarapu; Pal, Prem

    2014-01-01

    Silicon dioxide (SiO2) thin films are most commonly used insulating films in the fabrication of silicon-based integrated circuits (ICs) and microelectromechanical systems (MEMS). Several techniques with different processing environments have been investigated to deposit silicon dioxide films at temperatures down to room temperature. Anodic oxidation of silicon is one of the low temperature processes to grow oxide films even below room temperature. In the present work, uniform silicon dioxide thin films are grown at room temperature by using anodic oxidation technique. Oxide films are synthesized in potentiostatic and potentiodynamic regimes at large applied voltages in order to investigate the effect of voltage, mechanical stirring of electrolyte, current density and the water percentage on growth rate, and the different properties of as-grown oxide films. Ellipsometry, FTIR, and SEM are employed to investigate various properties of the oxide films. A 5.25 Å/V growth rate is achieved in potentiostatic mode. In the case of potentiodynamic mode, 160 nm thickness is attained at 300 V. The oxide films developed in both modes are slightly silicon rich, uniform, and less porous. The present study is intended to inspect various properties which are considered for applications in MEMS and Microelectronics. PMID:24672287

  3. In situ electrochemical investigation of tungsten electrochemical behavior during chemical mechanical polishing

    SciTech Connect

    Stein, D.J.; Cecchi, J.L.; Hetherington, D.; Guilinger, T.

    1998-09-01

    The electrochemical behavior of tungsten during chemical mechanical polishing (CMP) was observed in order to investigate a proposed blanket passivation and abrasion mechanism for tungsten removal. The experiments were performed in a cell that allowed electrochemical measurements to be made during polish. Polish rates were determined from the same samples used in the cell. Alumina-based polish slurries containing potassium iodate, ferric nitrate, or ammonium persulfate were used. DC polarization experiments show no evidence of passive film formation on the tungsten during polish. Tungsten oxidation rates measured during polish account for removal rates that are 1 to 2 orders of magnitude below the measured polish rate. Values of the charge-transfer resistance (measured by ac impedance spectroscopy) during polish are 1 to 2 orders of magnitude higher than expected from the polish rate, thus corroborating the dc-based data. Polish rates under potentiostatic conditions were also measured. The current required to maintain the metal anodic of the open-circuit potential is well below the current expected from measured polish rates, assuming complete oxidation of the tungsten. The polish rate during cathodic potentiostatic conditions ({minus}0.5 V with regard to the open-circuit potential) was similar to the polish rate at open circuit. The authors conclude that the formation of a blanket passive layer does not significantly contribute to tungsten removal during CMP.

  4. Effect of chemical composition on the corrosion behavior of Ni-Cr-Mo dental casting alloys.

    PubMed

    Huang, Her-Hsiung

    2002-06-01

    The objective of this investigation was to study the compositional influence on the corrosion behavior of Ni-Cr-Mo dental casting alloys in acidic artificial saliva. Cyclic potentiodynamic and potentiostatic tests were used to evaluate the corrosion behavior of different Ni-Cr-Mo dental casting alloys in deaerated artificial saliva with pH 5 at 37 degrees C. Optical microscope observations were made following the cyclic potentiodynamic tests. Surface chemical analyses were characterized by X-ray photoelectron spectroscopy and auger electron spectroscopy following the potentiostatic tests. The results show that the corrosion resistance of the Ni-Cr-Mo casting alloys investigated is associated with the formation of passive film containing Ni(OH)(2), NiO, Cr(2)O(3), and MoO(3), on the surface. The pitting potential and passive range, respectively, were statistically different among the different Ni-Cr-Mo alloys. The Ni-Cr-Mo alloys with higher Cr ( approximately 21%) and Mo ( approximately 8%) contents had a much larger passive range in the polarization curve and were immune to pitting corrosion due to the presence of high Cr (maximum approximately 31-35%) and Mo (maximum approximately 12%) contents in the surface passive film. The presence of Ti lower than 4% in the Ni-Cr-Mo casting alloy had no effect on corrosion resistance. A pitting resistance equivalent (PRE) of about 49 could provide the Ni-Cr-Mo alloy with a good pitting corrosion resistance. PMID:11920670

  5. TEM investigations on the local microstructure of electrodeposited galfenol nanowires

    NASA Astrophysics Data System (ADS)

    Pohl, D.; Damm, C.; Pohl, D.; Schultz, L.; Schlörb, H.

    2016-01-01

    The local microstructure of Fe-Ga nanowires is investigated considering dependence on the deposition technique. Using a complexed electrolyte, smooth and homogeneous Fe80Ga20 nanowires are deposited into anodic aluminum oxide templates by either applying pulse potential or potentiostatic deposition technique. At optimized deposition conditions the wires show the desired composition of Fe80±2Ga20±2 without a gradient along the growth direction. Composition distribution, structure and microstructure are examined in detail and reveal only minor differences. Line EELS and crystal lattice measurements reveal a negligible oxygen content for both preparation routines. Neither Fe/Ga oxides nor hydroxides were found. Both potentiostatically deposited as well as pulse deposited nanowires exhibit a preferred <110> orientation, the latter with slightly larger crystals. Different contrast patterns were found by TEM that appear more pronounced in the case of pulse deposited wires. High resolution transmission electron microscopy analysis and comparison of differently prepared focused ion beam lamellas reveal that these contrasts are caused by defects in the alternating potential deposition itself and are not induced during the TEM preparation process. The alternating potential mode causes periodic growth thereby inducing different layers with reduced wire thickness/defects at the layer interfaces.

  6. Miniaturized neural sensing and optogenetic stimulation system for behavioral studies in the rat

    NASA Astrophysics Data System (ADS)

    Kim, Min Hyuck; Nam, Ilho; Ryu, Youngki; Wellman, Laurie W.; Sanford, Larry D.; Yoon, Hargsoon

    2015-04-01

    Real time sensing of localized electrophysiological and neurochemical signals associated with spontaneous and evoked neural activity is critically important for understanding neural networks in the brain. Our goal is to enhance the functionality and flexibility of a neural sensing and stimulation system for the observation of brain activity that will enable better understanding from the level of individual cells to that of global structures. We have thus developed a miniaturized electronic system for in-vivo neurotransmitter sensing and optogenetic stimulation amenable to behavioral studies in the rat. The system contains a potentiostat, a data acquisition unit, a control unit, and a wireless data transfer unit. For the potentiostat, we applied embedded op-amps to build single potential amperometry for electrochemical sensing of dopamine. A light emitting diode is controlled by a microcontroller and pulse width modulation utilized to control optogenetic stimulation within a sub-millisecond level. In addition, this proto-typed electronic system contains a Bluetooth module for wireless data communication. In the future, an application-specific integrated circuit (ASIC) will be designed for further miniaturization of the system.

  7. Corrosion behaviour of austenitic stainless steel as a function of methanol concentration for direct methanol fuel cell bipolar plate

    NASA Astrophysics Data System (ADS)

    Wang, Lixia; Kang, Bin; Gao, Na; Du, Xiao; Jia, Linan; Sun, Juncai

    2014-05-01

    The corrosion behaviour of an AISI 304 stainless steel (304 SS) is investigated in aqueous acid methanol solutions (0.5 M H2SO4 + 2 ppm HF + x M CH3OH, x = 0, 1, 5, 10 and 20) at 50 °C to simulate the varied anodic operating conditions of direct methanol fuel cells. Electrochemical measurements including potentiodynamic polarisation, potentiostatic polarisation and electrochemical impedance spectroscopy tests, are employed to analyse the corrosion behaviour. The results reveal that the corrosion resistance of 304 SS is enhanced in solutions with higher methanol content. Scanning electron microscopy and inductively coupled plasma atomic emission spectrometry data indicate that the surface corrosion on 304 SS is alleviated when the methanol concentration is increased. According to the X-ray photoelectron spectroscopy and Mott-Schottky analyses, the passive films formed on the 304 SS after potentiostatic tests in all the test solutions are composed of a duplex electronic structure with an external n-type semiconductor layer and an internal p-type semiconductor layer. Further analyses of the surface conductivity conducted by measuring the interfacial contact resistance between the 304 SS and carbon paper reveal that the passive film formed in the solution with higher methanol content exhibits lower conductivity.

  8. Fabrication of the CuO/Cu2O heterojunction using an electrodeposition technique for solar cell applications

    NASA Astrophysics Data System (ADS)

    Wijesundera, R. P.

    2010-04-01

    Thin films of n-type cuprous oxide (Cu2O) were potentiostatically electrodeposited on a Ti substrate in an acetate bath. Cu2O thin films were annealed at 500 °C for 30 min in air for growing p-type cupric oxide (CuO) thin films. n-Cu2O thin films were potentiostatically electrodeposited in an acetate bath on Ti/CuO electrodes in order to fabricate the p-CuO/n-Cu2O heterojunction. The structural, morphological and optoelectronic properties of the CuO/Cu2O heterojunction were studied using x-ray diffraction (XRD), scanning electron micrographs (SEMs) and dark and light current-voltage characteristics. XRD and SEM reveal that well-covered single phase polycrystalline Cu2O thin film on the Ti/CuO electrode can be possible at the deposition potential of -550 mV versus the saturated calomel electrode (SCE) in an acetate bath. Photovoltaic characteristics further established the formation of the CuO/Cu2O heterojunction.

  9. Electrodeposition of Bi(x)Fe(1-x) intermetallic compound nanowire arrays and their magnetic properties.

    PubMed

    Li, Gao-Ren; Tong, Ye-Xiang; Kay, Lin-Gang; Liu, Guan-Kun

    2006-05-11

    There have been few reports on Bi-Fe intermetallic compounds because Bi and Fe are immiscible in the equilibrium states and neither alloy nor intermetallic compound exists in the binary system. In this paper, we show that, by using the nanometer-scale templates based synthesis in conjunction with the electrochemical deposition, it is possible to mix in solid solution elements that are immiscible in traditional fabrication methods. The preparation of Bi-Fe intermetallic compound nanowire arrays was investigated via an electrodeposition route by using a polycarbonate (PC) membrane template. Cyclic voltammetry, potentiostatic transient, and potentiostatic stripping were used to study the formation of Bi(x)Fe(1-x) intermetallic compounds. The compositions of Bi(1-x)Fe(x) intermetallic compound nanowire arrays were sensitive to the bath compositions and the electrodeposition potentials, and the length could be easily adjusted by varying the electrodeposition time. The electrodeposited Bi(1-x)Fe(x) intermetallic compound nanowire arrays had a parallel-to-the-wire easy magnetization. Furthermore, the spin-glass such as behavior and an unusually large characteristic time, which was about 5.26 h, were found in Bi(1-x)Fe(x) intermetallic compound nanowire arrays at room temperature. PMID:16671702

  10. Waste water derived electroactive microbial biofilms: growth, maintenance, and basic characterization.

    PubMed

    Gimkiewicz, Carla; Harnisch, Falk

    2013-01-01

    The growth of anodic electroactive microbial biofilms from waste water inocula in a fed-batch reactor is demonstrated using a three-electrode setup controlled by a potentiostat. Thereby the use of potentiostats allows an exact adjustment of the electrode potential and ensures reproducible microbial culturing conditions. During growth the current production is monitored using chronoamperometry (CA). Based on these data the maximum current density (jmax) and the coulombic efficiency (CE) are discussed as measures for characterization of the bioelectrocatalytic performance. Cyclic voltammetry (CV), a nondestructive, i.e. noninvasive, method, is used to study the extracellular electron transfer (EET) of electroactive bacteria. CV measurements are performed on anodic biofilm electrodes in the presence of the microbial substrate, i.e. turnover conditions, and in the absence of the substrate, i.e. nonturnover conditions, using different scan rates. Subsequently, data analysis is exemplified and fundamental thermodynamic parameters of the microbial EET are derived and explained: peak potential (Ep), peak current density (jp), formal potential (E(f)) and peak separation (ΔEp). Additionally the limits of the method and the state-of the art data analysis are addressed. Thereby this video-article shall provide a guide for the basic experimental steps and the fundamental data analysis. PMID:24430581

  11. Electrochemical behaviour of silver in borate buffer solutions

    NASA Astrophysics Data System (ADS)

    Zaky, Ayman M.; Assaf, Fawzi H.; Abd El Rehim, Sayed S.; Mohamed, Basheer M.

    2004-01-01

    The electrochemical behaviour of Ag in aqueous 0.15 M borax and 0.15 M boric acid buffer solution was studied under various conditions using cyclic voltammetry and potentiostatic techniques. It was found that the anodic polarization curve of Ag in borate buffer solution was characterized by the appearance of two potential regions, active and passive, prior to the oxygen evolution reaction. The active potential region was characterized by the appearance of three anodic peaks, the first two peaks A 1 and A 2 correspond to the oxidation of Ag and formation of [Ag(OH) 2] - soluble compound and a passive film of Ag 2O on the electrode surface. The third anodic peak corresponds to the conversion of both [Ag(OH) 2] - and Ag 2O to Ag 2O 2. X-ray diffraction patterns confirmed the existence of Ag 2O and Ag 2O 2 passive layers on the electrode surface potentiodynamically polarized up to 800 mV. Potentiostatic current transient measurements showed that the formation of Ag 2O and Ag 2O 2 involves a nucleation and growth mechanism under diffusion control.

  12. Simplifying microbial electrosynthesis reactor design

    PubMed Central

    Giddings, Cloelle G. S.; Nevin, Kelly P.; Woodward, Trevor; Lovley, Derek R.; Butler, Caitlyn S.

    2015-01-01

    Microbial electrosynthesis, an artificial form of photosynthesis, can efficiently convert carbon dioxide into organic commodities; however, this process has only previously been demonstrated in reactors that have features likely to be a barrier to scale-up. Therefore, the possibility of simplifying reactor design by both eliminating potentiostatic control of the cathode and removing the membrane separating the anode and cathode was investigated with biofilms of Sporomusa ovata. S. ovata reduces carbon dioxide to acetate and acts as the microbial catalyst for plain graphite stick cathodes as the electron donor. In traditional ‘H-cell’ reactors, where the anode and cathode chambers were separated with a proton-selective membrane, the rates and columbic efficiencies of microbial electrosynthesis remained high when electron delivery at the cathode was powered with a direct current power source rather than with a potentiostat-poised cathode utilized in previous studies. A membrane-less reactor with a direct-current power source with the cathode and anode positioned to avoid oxygen exposure at the cathode, retained high rates of acetate production as well as high columbic and energetic efficiencies. The finding that microbial electrosynthesis is feasible without a membrane separating the anode from the cathode, coupled with a direct current power source supplying the energy for electron delivery, is expected to greatly simplify future reactor design and lower construction costs. PMID:26029199

  13. Role of minor alloying elements on the performance of lead/acid battery grids. Part 2. Corrosion of lead-arsenic alloys

    NASA Astrophysics Data System (ADS)

    Gad Allah, A. G.; Abd El-Rahman, H. A.; Abd El-Galil, M.

    Corrosion of PbAs alloys (As = 0.1, 0.2, 0.3 and 0.4%) in 5.0 M H 2SO 4 solutions at 30°C was studied under open-circuit, potentiostatic and galvanostatic polarization conditions. The sulfation process under open-circuit conditions increased as the As concentration increased and the open-circuit potential shifted to more cathodic values. The presence of As affected significantly the potentiostatic polarization curve and caused a substantial decrease in passivity current and increased the overpotentials of both the O 2- and the H 2-evolution reactions. The self-discharging process decreased as the concentration of As increased with formation of substantial amounts of lead oxide beside PbSO 4. When PbAs alloys were subjected to alternative cathodic and anodic galvanostatic polarization cycles, the corrodable layer thickness increased in the order of: Pb-0.1%As>Pb-0.3%As%>Pb-0.4%As>Pb>Pb-0.2%As. The efficiency of PbO 2 formation also depended on the percentage As.

  14. Growth and Etch Rate Study of Low Temperature Anodic Silicon Dioxide Thin Films

    PubMed Central

    Ashok, Akarapu; Pal, Prem

    2014-01-01

    Silicon dioxide (SiO2) thin films are most commonly used insulating films in the fabrication of silicon-based integrated circuits (ICs) and microelectromechanical systems (MEMS). Several techniques with different processing environments have been investigated to deposit silicon dioxide films at temperatures down to room temperature. Anodic oxidation of silicon is one of the low temperature processes to grow oxide films even below room temperature. In the present work, uniform silicon dioxide thin films are grown at room temperature by using anodic oxidation technique. Oxide films are synthesized in potentiostatic and potentiodynamic regimes at large applied voltages in order to investigate the effect of voltage, mechanical stirring of electrolyte, current density and the water percentage on growth rate, and the different properties of as-grown oxide films. Ellipsometry, FTIR, and SEM are employed to investigate various properties of the oxide films. A 5.25 Å/V growth rate is achieved in potentiostatic mode. In the case of potentiodynamic mode, 160 nm thickness is attained at 300 V. The oxide films developed in both modes are slightly silicon rich, uniform, and less porous. The present study is intended to inspect various properties which are considered for applications in MEMS and Microelectronics. PMID:24672287

  15. Electrochemical reaction of lithium with nanosized vanadium antimonate

    SciTech Connect

    Morales, Julian; Sanchez, Luis . E-mail: luis-sanchez@uco.es; Martin, Francisco; Berry, Frank

    2006-08-15

    Nanometric vanadium antimonate, VSbO{sub 4}, was prepared by mechanical milling from Sb{sub 2}O{sub 3} and V{sub 2}O{sub 5} and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Mossbaueer spectroscopy (MS) and X-ray photoelectron spectroscopy (XPS) techniques. Its reactivity towards lithium was examined by testing Li/VSbO{sub 4} cells under galvanostatic and potentiostatic regimes. The amount of Li inserted was found to be consistent with a two-step process involving the reactions (i) VSbO{sub 4}+8 Li{sup {yields}}Sb+V+4 Li{sub 2}O and (ii) Sb+3 Li{sup {yields}}Li{sub 3}Sb, the former being virtually irreversible and the latter reversible as suggested by the shape of the anodic and cathodic curves. Ex situ XPS measurements of the discharged and charged electrode provided direct evidence of the formation of alloyed Sb and confirmed the results of the potentiostatic curves regarding the irreversible or reversible character of the previous reactions. The Li/VSbO{sub 4} cell exhibited acceptable electrochemical performance, which surpassed that of other Sb-based compounds as the likely result of the formation of V and its associated enhanced electrode conductivity. - Graphical abstract: TEM image of nanosized VSbO{sub 4} sample.

  16. Scanning electron microscope studies on the breakdown of passivity of a nickel-chromium-molybdenum dental alloy.

    PubMed

    Geis-Gerstorfer, J; Göpel, W; Weber, H

    1987-09-01

    The breakdown of passivity and localized corrosion of a Ni-20Cr-10Mo alloy was investigated. The methods employed were potentiodynamic polarization and SEM, and AES and EDX after potentiostatic polarization over a period of 20 hours in the passive and transpassive regions. The 1 micron finished as-cast specimens were polarized in aerated 0.1 M NaCl. The cyclic polarization curves revealed a critical pitting potential of 470 mV (SCE), while the protection potential was 300 mV (SCE). Using the potentiostatic polarization technique, nearly constant corrosion currents appeared, indicating that the whole surface was corroded uniformly. SEM pictures of samples, corroded at 650 mV, showed little pits under the oxide layer and a thinning down of the outer oxide layer. This lead to the opinion that the penetration as well as the adsorption mechanism determine the breakdown of passivity. EDX analysis and AES depth profiles showed an enrichment of Cr and Mo in the oxide. In contrast to oxidized samples, no second layer of Ni was found in the outer oxide region. In the transpassive region the relative amount of Cr and Mo in the oxide layer was higher than the one found in corresponding samples polarized in the passive region. The oxide thickness found was about 5 nm in the passive region (300 mV SCE) and about 250 nm in the transpassive region (650 mV SCE). PMID:3659856

  17. Investigation of corrosion and stability of lead-brass alloy in acid and neutral solutions using electrochemical impedance spectroscopy

    SciTech Connect

    Badawy, W.A.; El-Egamy, S.S.; Azab, A.S.

    1997-11-01

    The corrosion behavior of a lead-brass alloy (58% Cu, 1.8% Pb, and 42.2% Zn) was investigated in naturally aerated acid and neutral chloride and sulfate solutions under open-circuit and potentiostatic control conditions using electrochemical impedance spectroscopy (EIS). Corrosion under open-circuit conditions was caused mainly by the dissolved oxygen depolarizer, copper (I) chloride (CuCl) or copper (I) sulfate (Cu{sub 2}SO{sub 4}), together with some surface oxides, which were assumed to be corrosion products, leading to electrode passivation. Impedance spectra in the form of Nyquist plots consisted of depressed semicircles with different degrees of depression. These depressions increased with dilution of the electrolyte rather than with immersion time. This behavior was attributed partially to inhomogeneities and surface roughness. Data were analyzed in terms of the constant phase element model, which reduced to infinite Warburg diffusion in neutral solutions. At high cathodic overpotentials, reduction of hydrogen (H{sup +}) in acid media and of oxygen in neutral media seemed to be rate controlling. Potentiostatic polarization at potentials > {minus}0.5 V led to selective dissolution of zinc and accumulation of corrosion products. At potentials > {minus}0.2 V, pitting occurred.

  18. Simplifying microbial electrosynthesis reactor design.

    PubMed

    Giddings, Cloelle G S; Nevin, Kelly P; Woodward, Trevor; Lovley, Derek R; Butler, Caitlyn S

    2015-01-01

    Microbial electrosynthesis, an artificial form of photosynthesis, can efficiently convert carbon dioxide into organic commodities; however, this process has only previously been demonstrated in reactors that have features likely to be a barrier to scale-up. Therefore, the possibility of simplifying reactor design by both eliminating potentiostatic control of the cathode and removing the membrane separating the anode and cathode was investigated with biofilms of Sporomusa ovata. S. ovata reduces carbon dioxide to acetate and acts as the microbial catalyst for plain graphite stick cathodes as the electron donor. In traditional 'H-cell' reactors, where the anode and cathode chambers were separated with a proton-selective membrane, the rates and columbic efficiencies of microbial electrosynthesis remained high when electron delivery at the cathode was powered with a direct current power source rather than with a potentiostat-poised cathode utilized in previous studies. A membrane-less reactor with a direct-current power source with the cathode and anode positioned to avoid oxygen exposure at the cathode, retained high rates of acetate production as well as high columbic and energetic efficiencies. The finding that microbial electrosynthesis is feasible without a membrane separating the anode from the cathode, coupled with a direct current power source supplying the energy for electron delivery, is expected to greatly simplify future reactor design and lower construction costs. PMID:26029199

  19. An electrochromic film device to teach polymer electrochemical physics

    NASA Astrophysics Data System (ADS)

    Huang, Mei-Rong; Tao, Tao; Li, Xin-Gui; Gong, Qian-Cheng

    2007-09-01

    We discuss the background associated with an electrochromic device that can reversibly change its color and optical density at a specific potential. We discuss the underlying science needed to make a new polyaniline (PAN)/polyvinyl alcohol(PVA) electrochromic composite film on an indium-tin oxide (ITO) conducting glass by electropolymerization and describe a reversible redox transition of the PAN. The experiment gives students an opportunity to fabricate an electrochromic device containing PAN, one of the most important conducting polymers. The experimental conditions are flexible so that each group of students can construct their own electrochromic device with particular behavior. Two techniques for polymerizing the PAN and three methods of demonstrating the electrochromism are given, depending on the available apparatus. A sophisticated three-electrode potentiostat or a crude apparatus containing a battery, wire, a variable resistor, and a voltage meter is used to synthesize the PAN deposit. The electrochromic property is repetitively observed by reversibly changing the applied potentials on the device. A potentiostatic apparatus, a single flashlight battery, or a flashlight battery accompanied by a variable resistor allows students to observe multicolor electrochromism. The experiments significantly enhance students' understanding of polymer chemicophysics principles and their appreciation of novel variable colorful films. The experiments are safe and easy to perform, provided that appropriate precautions are taken.

  20. Origins of nanoscale damage to glass-sealed platinum electrodes with submicrometer and nanometer size.

    PubMed

    Nioradze, Nikoloz; Chen, Ran; Kim, Jiyeon; Shen, Mei; Santhosh, Padmanabhan; Amemiya, Shigeru

    2013-07-01

    Glass-sealed Pt electrodes with submicrometer and nanometer size have been successfully developed and applied for nanoscale electrochemical measurements such as scanning electrochemical microscopy (SECM). These small electrodes, however, are difficult to work with because they often lose a current response or give a low SECM feedback in current-distance curves. Here we report that these problems can be due to the nanometer-scale damage that is readily and unknowingly made to the small tips in air by electrostatic discharge or in electrolyte solution by electrochemical etching. The damaged Pt electrodes are recessed and contaminated with removed electrode materials to lower their current responses. The recession and contamination of damaged Pt electrodes are demonstrated by scanning electron microscopy and X-ray energy dispersive spectroscopy. The recessed geometry is noticeable also by SECM but is not obvious from a cyclic voltammogram. Characterization of a damaged Pt electrode with recessed geometry only by cyclic voltammetry may underestimate electrode size from a lower limiting current owing to an invalid assumption of inlaid disk geometry. Significantly, electrostatic damage can be avoided by grounding a Pt electrode and nearby objects, most importantly, an operator as a source of electrostatic charge. Electrochemical damage can be avoided by maintaining potentiostatic control of a Pt electrode without internally disconnecting the electrode from a potentiostat between voltammetric measurements. Damage-free Pt electrodes with submicrometer and nanometer sizes are pivotal for reliable and quantitative nanoelectrochemical measurements. PMID:23763642

  1. Amperometric measurements of ethanol on paper with a glucometer.

    PubMed

    Wu, Grace; Zaman, Muhammad H

    2015-03-01

    Recent advances in electrochemical analysis on filter paper exemplify the versatility of this substrate for high performance testing. Its low-cost, light-weight, and environmentally friendly properties make it particularly attractive for applications in addressing health and environmental safety needs in low-resource settings and developing countries. However, the main drawback to sensitive electrochemical testing is the use of a potentiostat, a bench-top instrument that is extremely expensive, thereby negating the some of the benefits of paper-based devices. Hence there is a need to develop paper-devices for use with handheld, portable device readers that can extract quantitative readouts. In this study, we developed a method to use micro-paper electrochemical devices, or µPEDs, with a glucose meter, which are used for personal monitoring of blood glucose levels. Ethanol was chosen as a model target analyte due to its importance in the global issue of road safety. µPEDs were simple in design and could be tested with a potentiostat. We observed that inclusion of the stabilizer trehalose was critical to preparing µPEDs for later analysis. In addition, an NAD(+)-dependent enzyme was used to impart selectivity to the biosensor, which also represents a class of enzymes with targets relevant to the health and food industry. PMID:25618657

  2. Integrated Nanopore Detectors in a Standard Complementary Metal-Oxide-Semiconductor Process

    NASA Astrophysics Data System (ADS)

    Uddin, Ashfaque; Chen, Chin-Hsuan; Yemenicioglu, Sukru; Milaninia, Kaveh; Corigliano, Ellie; Varma, Madoo; Theogarajan, Luke

    2012-02-01

    High-bandwidth and low-noise nanopore sensor and detection electronics are crucial in achieving single-DNA base resolution. A potential way to accomplish this goal is to integrate solid-state nanopores within a CMOS platform, in close proximity to the biasing electrodes and custom-designed amplifier electronics. Here we report the development of solid-state nanopore devices in a commercial CMOS potentiostat chip implemented in On-Semiconductor's 0.5 micron technology. By using post-CMOS micromachining, a free-standing oxide membrane and electrodes are fabricated utilizing the N+ polysilicon/oxide/N+ polysilicon capacitor structure available in the aforementioned process. Nanopores with sub-5 nm diameter are drilled in the membrane using a Transmission Electron Microscope. The integrity of pores is validated by measuring current-voltage and noise characteristics. DNA translocation experiments are also performed utilizing these on-chip pores. In addition, electrical tests performed on the CMOS potentiostat circuitry show that the post-CMOS micromachining process does not have any detrimental effect on the CMOS circuitry.

  3. An Approach to an Inhibition Electronic Tongue to Detect On-Line Organophosphorus Insecticides Using a Computer Controlled Multi-Commuted Flow System

    PubMed Central

    Alonso, Gustavo A.; Dominguez, Rocio B.; Marty, Jean-Louis; Muñoz, Roberto

    2011-01-01

    An approach to an inhibition bioelectronic tongue is presented. The work is focused on development of an automated flow system to carry out experimental assays, a custom potentiostat to measure the response from an enzymatic biosensor, and an inhibition protocol which allows on-line detections. A Multi-commuted Flow Analysis system (MCFA) was selected and developed to carry out assays with an improved inhibition method to detect the insecticides chlorpyrifos oxon (CPO), chlorfenvinfos (CFV) and azinphos methyl-oxon (AZMO). The system manifold comprised a peristaltic pump, a set of seven electronic valves controlled by a personal computer electronic interface and software based on LabView® to control the sample dilutions into the cell. The inhibition method consists in the injection of the insecticide when the enzyme activity has reached the plateau of the current; with this method the incubation time is avoided. A potentiostat was developed to measure the response from the enzymatic biosensor. Low limits of detection of 10 nM for CPO, CFV, and AZMO were achieved. PMID:22163822

  4. An approach to an inhibition electronic tongue to detect on-line organophosphorus insecticides using a computer controlled multi-commuted flow system.

    PubMed

    Alonso, Gustavo A; Dominguez, Rocio B; Marty, Jean-Louis; Muñoz, Roberto

    2011-01-01

    An approach to an inhibition bioelectronic tongue is presented. The work is focused on development of an automated flow system to carry out experimental assays, a custom potentiostat to measure the response from an enzymatic biosensor, and an inhibition protocol which allows on-line detections. A Multi-commuted Flow Analysis system (MCFA) was selected and developed to carry out assays with an improved inhibition method to detect the insecticides chlorpyrifos oxon (CPO), chlorfenvinfos (CFV) and azinphos methyl-oxon (AZMO). The system manifold comprised a peristaltic pump, a set of seven electronic valves controlled by a personal computer electronic interface and software based on LabView® to control the sample dilutions into the cell. The inhibition method consists in the injection of the insecticide when the enzyme activity has reached the plateau of the current; with this method the incubation time is avoided. A potentiostat was developed to measure the response from the enzymatic biosensor. Low limits of detection of 10 nM for CPO, CFV, and AZMO were achieved. PMID:22163822

  5. Three-Dimensional Growth of Li2S in Lithium-Sulfur Batteries Promoted by a Redox Mediator.

    PubMed

    Gerber, Laura C H; Frischmann, Peter D; Fan, Frank Y; Doris, Sean E; Qu, Xiaohui; Scheuermann, Angelique M; Persson, Kristin; Chiang, Yet-Ming; Helms, Brett A

    2016-01-13

    During the discharge of a lithium-sulfur (Li-S) battery, an electronically insulating 2D layer of Li2S is electrodeposited onto the current collector. Once the current collector is enveloped, the overpotential of the cell increases, and its discharge is arrested, often before reaching the full capacity of the active material. Guided by a new computational platform known as the Electrolyte Genome, we advance and apply benzo[ghi]peryleneimide (BPI) as a redox mediator for the reduction of dissolved polysulfides to Li2S. With BPI present, we show that it is now possible to electrodeposit Li2S as porous, 3D deposits onto carbon current collectors during cell discharge. As a result, sulfur utilization improved 220% due to a 6-fold increase in Li2S formation. To understand the growth mechanism, electrodeposition of Li2S was carried out under both galvanostatic and potentiostatic control. The observed kinetics under potentiostatic control were modeled using modified Avrami phase transformation kinetics, which showed that BPI slows the impingement of insulating Li2S islands on carbon. Conceptually, the pairing of conductive carbons with BPI can be viewed as a vascular approach to the design of current collectors for energy storage devices: here, conductive carbon "arteries" dominate long-range electron transport, while BPI "capillaries" mediate short-range transport and electron transfer between the storage materials and the carbon electrode. PMID:26691496

  6. Wearable electrochemical sensors for in situ analysis in marine environments.

    PubMed

    Malzahn, Kerstin; Windmiller, Joshua Ray; Valdés-Ramírez, Gabriela; Schöning, Michael J; Wang, Joseph

    2011-07-21

    The development of wearable screen-printed electrochemical sensors on underwater garments comprised of the synthetic rubber neoprene is reported. These wearable sensors are able to determine the presence of environmental pollutants and security threats in marine environments. Owing to its unique elastic and superhydrophobic morphology, neoprene is an attractive substrate for thick-film electrochemical sensors for aquatic environments and offers high-resolution printing with no apparent defects. The neoprene-based sensor was evaluated for the voltammetric detection of trace heavy metal contaminants and nitroaromatic explosives in seawater samples. We also describe the first example of enzyme (tyrosinase) immobilization on a wearable substrate towards the amperometric biosensing of phenolic contaminants in seawater. Furthermore, the integration of a miniaturized potentiostat directly on the underwater garment is demonstrated. The wearable sensor-potentiostat microsystem provides a visual indication and alert if the levels of harmful contaminants have exceeded a pre-defined threshold. The concept discussed here is well-suited for integration into dry- and wetsuits worn by divers and recreational surfers/swimmers, thereby providing them with the ability to continuously assess their surroundings for environmental contaminants and security hazards. PMID:21637863

  7. Facile production of thermoelectric bismuth telluride thick films in the presence of polyvinyl alcohol.

    PubMed

    Lei, C; Burton, M R; Nandhakumar, I S

    2016-06-01

    Bismuth telluride is currently the best performing thermoelectric material for room temperature operations in commercial thermoelectric devices. We report the reproducible and facile production of 600 micron thick bismuth telluride (Bi2Te3) layers by low cost and room temperature pulsed and potentiostatic electrodeposition from a solution containing bismuth and tellurium dioxide in 2 M nitric acid onto nickel in the presence of polyvinyl alcohol (PVA). This was added to the electrolyte to promote thick layer formation and its effect on the structure, morphology and composition of the electrodeposits was investigated by SEM and EDX. Well adherent, uniform, compact and stoichiometric n-type Bi2Te3 films with a high Seebeck coefficient of up to -200 μV K(-1) and a high electrical conductivity of up to 400 S cm(-1) resulting in a power factor of 1.6 × 10(-3) W m(-1) K(-2) at film growth rates of 100 μm h(-1) for potentiostatic electrodeposition were obtained. The films also exhibited a well defined hexagonal structure as determined by XRD. PMID:27166737

  8. Physical characterization of ultrathin anodic silicon oxide films

    NASA Astrophysics Data System (ADS)

    Clark, K. B.; Bardwell, J. A.; Baribeau, J.-M.

    1994-09-01

    Ultrathin oxides formed on p-type (100) Si using anodic oxidation in dilute aqueous NH4OH solution have been characterized by Fourier transform infrared spectroscopy (FITR), x-ray photoelectron spectroscopy (XPS), and x-ray reflectomery. The aim of the work was to optimize the growth and annealing conditions for fabrication of ultrathin gate oxides. Two alternate growth conditions (potentiostatic and galvanostatic) could be used to grow oxides of thickness between 3 and 16 nm. There was very little difference between the two types of oxides; however, the FTIR asymmetric stretch maximum nu(sub m) was at slightly higher frequencies and this band was slightly narrower for potentiostatic oxides compared to galvanostatic oxides of the same thickness. For both types of films, nu(sub m) increased with film thickness, while the corresponding full width at half-maximum decrease. As-grown approximately 11nm-thick films of both types contain 3.8 +/- 0.3% -OH (bound as isolated silanol) and 5.0 +/- 0.4% -OH (bound as H2O and/or associated silanol) by mass, and have a density of 2.05 +/- 0.03 g/cu cm compared with a density of 2.27 +/- 0.03 g/cu cm measured for thermal oxides. Thus, the composition of the as-grown anodic oxides can be written as SiO(1.93)(OH)(0.14)-0.18H2O. Discounting the H content, this converts to an O/Si ratio of 2.25 +/- 0.02, which can be compared to the O/Si ratio of 2.27 +/- 0.06 measured for as-grown films by XPS. Potentiostatically grown approximately 11-nm-thick films were annealed at temperatures between 300 and 900 C in forming gas. Two different stages were observed as a function of annela temperature. At temperatures below 500 C, water and/or associated silanol was ejected from the films. This resulted in a maximum in the stress and/or disorder in the oxides at anneal temperatures of 500 C. At temperatures above 500 C, the remainder of the silanol was removed from the films; some kind of stress relief occurred. The oxides became stoichiometric at temperatures 700 C and above.

  9. Design of a miniaturized electrochemical instrument for in-situ O2 monitoring

    NASA Astrophysics Data System (ADS)

    Colomer-Farrarons, Jordi; Miribel-Català, Pedro L.; Samitier, Josep; Arundell, Martin; Rodríguez, Ivón

    2009-05-01

    The authors are working toward the design of a device for the detection of oxygen, following a discrete and an integrated instrumentation implementation. The discrete electronics are also used for preliminary analysis, to confirm the validity of the conception of system, and its set-up would be used in the characterization of the integrated device, waiting for the chip fabrication. This paper presents the design of a small and portable potentiostat integrated with electrodes, which is cheap and miniaturized, which can be applied for on-site measurements for the simultaneous detection of O2 and temperature in water systems. As a first approach a discrete PCB has been designed based on commercial discrete electronics and specific oxygen sensors. Dissolved oxygen concentration (DO) is an important index of water quality and the ability to measure the oxygen concentration and temperature at different positions and depths would be an important attribute to environmental analysis. Especially, the objective is that the sensor and the electronics can be integrated in a single encapsulated device able to be submerged in environmental water systems and be able to make multiple measurements. For our proposed application a small and portable device is developed, where electronics and sensors are miniaturized and placed in close proximity to each other. This system would be based on the sensors and electronics, forming one module, and connected to a portable notebook to save and analyze the measurements on-line. The key electronics is defined by the potentiostat amplifier, used to fix the voltage between the Working (WE) and Reference (RE) electrodes following an input voltage (Vin). Vin is a triangular signal, programmed by a LabViewinterface, which is also used to represent the CV transfers. To obtain a smaller and compact solution the potentiostat amplifier has also been integrated defining a full custom ASIC amplifier, which is in progress, looking for a point-of-care device. These circuits have been designed with a 0.13 μm technology from ST Microelectronics through the CMP-TIMA service.

  10. The effect of deposition electrolyte on polypyrrole surface interaction with biological environment

    NASA Astrophysics Data System (ADS)

    Mîndroiu, Mihaela; Ungureanu, Camelia; Ion, Raluca; Pîrvu, Cristian

    2013-07-01

    The effects of electrolyte type used in electrodeposition of polypyrrole (PPy) films on Ti6Al7Nb alloy was studied in order to design a titanium modified surface with enhanced antibacterial activity and better biocompatibility. Therefore, the polypyrrole coatings were synthesized by potentiostatic electrochemically technique from pyrrole and lithium perchlorate (LiClO4) using aqueous and non-aqueous solutions. The both PPy films were characterized by electrochemical methods in Hank's Balanced Salt Solution (HBSS), and surface characterization by Atomic Force Microscopy (AFM) and Scanning Electron Microscopy (SEM) analysis, adhesion test and contact angle measurements. A correlation between the film stability and surface properties, synthesis parameters and the interaction with biological environment was established. The physical-chemical properties of the studied PPy films are in direct related with the doping level and have an important influence of the biocompatibility and antibacterial activity.

  11. Electrochemical behavior of 0.2 to 3 molar ferrous chloride-ferric chloride mixtures on edge-on pyrolytic graphite rotated disk electrodes

    NASA Technical Reports Server (NTRS)

    Miller, R. O.

    1977-01-01

    Potentiostatic determinations in various mixtures of FeCl2-FeCl3 with excess HCl show rest potentials that are 0.1 V less electropositive than the theoretical values from the formulated ratios of FeII to FeIII (probably as a result of complexing). The standard rate constant sub s. ranges between 0.0001 and 0.000 cm/sec. Tafel slopes b of roughly 0.12V per decade indicate single-electron exchange kinetics. No significant trend in either b or sub s was attributed to mixture composition. The higher sub s. values occurred with and edge-on pyrolytic graphite that had undergone a permanent surface change.

  12. Photoelectrochemical and Electrochemical Characterization of Sub-Micro-Gram Amounts of Organic Semiconductors Using Scanning Droplet Cell Microscopy

    PubMed Central

    2014-01-01

    A model organic semiconductor (MDMO-PPV) was used for testing a modified version of a photoelectrochemical scanning droplet cell microscope (PE-SDCM) adapted for use with nonaqueous electrolytes and containing an optical fiber for localized illumination. The most attractive features of the PE-SDCM are represented by the possibility of addressing small areas on the investigated substrate and the need of small amounts of electrolyte. A very small amount (ng) of the material under study is sufficient for a complete electrochemical and photoelectrochemical characterization due to the scanning capability of the cell. The electrochemical behavior of the polymer was studied in detail using potentiostatic and potentiodynamic investigations as well as electrochemical impedance spectroscopy. Additionally, the photoelectrochemical properties were investigated under illumination conditions, and the photocurrents found were at least 3 orders of magnitude higher than the dark (background) current, revealing the usefulness of this compact microcell for photovoltaic characterizations. PMID:25101149

  13. Measurement of Li/sup +/ ion transport numbers in PEO-LiX complexes. Technical report No. 16, 15 July 1985-January 1988

    SciTech Connect

    Munshi, M.Z.; Owens, B.B.; Nguyen, S.

    1988-03-01

    Lithium-ion conducting-polymer materials are being intensively investigated in a number of research laboratories because of their potential use as solid electrolytes in high-energy-density solid-state lithium batteries. The most-widely used polymer were based on polyethylene oxide (PEO). The conduction mechanism in these polymer electrolytes has generally been assumed to be due to Li(+)ion transport from one lone pair site to another along the helical PEO strands. However, recent studies have shown that the Li(+) transport number is less than unity. The transport number for Li(+) ions in PEO-LiX complexes was measured using a potentiostatic polarization technique. The results indicate that the Li(+) ion transport is strongly influenced by the salt concentration and the type of counter ions.

  14. Crevice corrosion products of dental amalgam

    SciTech Connect

    Sutow, E.J.; Jones, D.W.; Hall, G.C.; Owen, C.G. )

    1991-07-01

    The objective of this study was to determine the in vitro corrosion products that resulted from crevice corrosion of low- and high-copper dental amalgams. Specimens were potentiostatically polarized in a chloride-containing electrolyte while set against a PTFE surface to form a crevice. After 16 h, corrosion products were examined by light microscopy, SEM, EDS, and XRD. Analysis showed the presence of three previously reported products (Sn4(OH)6Cl2, SnO, and Cu2O) and a new product, CuCl, which formed on high-copper, {gamma} 2-free amalgams. Thermodynamic considerations show that CuCl is stable for the reported in vivo potentials of amalgam restorations and the high acidity and high chloride ion concentration associated with crevice corrosion.

  15. Copper electrocrystallization on titanium electrodes: Controlled growth of copper nuclei using a potential step technique

    NASA Astrophysics Data System (ADS)

    Sáez, V.; Graves, J.; Paniwnyk, L.; Mason, T. J.

    2010-01-01

    Copper nanoparticles were synthesized using a pulsed sonoelectrochemical (20 kHz, 78 Wcm-2) method. Two electrolytes used were a copper salt dissolved in Na2SO4 (pH=3.80) or H2SO4 (pH=0.6). For both electrolytes and in the absence of any surfactant, monodispersed spherical copper nanoparticles were strongly aggregated in three-dimensional clusters of about 200nm. The particle size is controlled by varying reaction parameters such as duration of the experiment, current density, temperature and ultrasound power. A potential step technique is proposed to synthesize copper nanoparticules. Under potentiostatic conditions the aim is to control and decrease the nanoparticle size and reduce production costs by avoiding gas evolution and other adverse reactions.

  16. The electrochemical behaviour of 316L austenitic stainless steel in Cl- containing environment under different H2S partial pressures

    NASA Astrophysics Data System (ADS)

    Ding, Jinhui; Zhang, Lei; Lu, Minxu; Wang, Jing; Wen, Zhibin; Hao, Wenhui

    2014-01-01

    In oil-gas production environments, presence of H2S-Cl- can induce deterioration of the passive film, leading to pitting corrosion of stainless steels. In this paper, by using potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) and capacitance measurements (Mott-Schottky analysis), the electrochemical behaviour of AISI 316L austenitic stainless steel was investigated in Cl- solutions under different H2S partial pressures (from 0 to 1.0 bar). The results indicated that presence of H2S in Cl- solution can accelerate both the cathodic and anodic current density, leading to a metastable passive state in higher passive potential range, changing the semiconductor behaviour from p-type to n-type, increasing its susceptibility to corrosion. XPS analysis was employed to characterize the surface film after potentiostatic polarization, whose results provide good evidences for the electrochemical measurements.

  17. Electrochemical Behavior of CrN Coated on 316L Stainless Steel in Simulated Cathodic Environment of Proton Exchange Membrane Fuel Cell

    NASA Astrophysics Data System (ADS)

    Nam, Nguyen Dang; Kim, Jung-Gu

    2008-08-01

    Four types of CrN coating were deposited on type 316L stainless steel by magnetron sputtering physical vapor deposition (PVD) for use in bipolar plates. Four samples deposited at various bias voltages were evaluated under potentiodynamic, potentiostatic, and electrochemical impedance spectroscopy (EIS) conditions. EIS data were monitored for 96 h in an aerated corrosive environment at 70 °C to determine coating performance at +600 mV application. The electrochemical behavior of the coatings was enhanced with decreasing bias voltage. The CrN films on the 316L stainless steel substrate exhibited high protective efficiency, that is, increasing corrosion resistance with decreasing bias voltage. X-ray diffraction (XRD) analysis confirmed the formation of crystalline-refined CrN(200) at a low bias voltage.

  18. SnO2-Based Gas (Methane) Anodes for Electrowinning of Aluminum

    NASA Astrophysics Data System (ADS)

    Xiao, S.; Mokkelbost, T.; Paulsen, O.; Ratvik, A. P.; Haarberg, Geir Martin

    2013-10-01

    SnO2-based and carbon-based gas anodes were studied in molten Na3AlF6-AlF3-Al2O3 at 1123 K (850 °C) for aluminum electrolysis. Methane was introduced to the porous anodes to take part in a three-phase (anode/electrolyte/methane) boundary reaction. Carbon was used as the cathode. It was observed that the anode potential was reduced by 0.6 V and that the current was increased up to three times in galvanostatic and potentiostatic tests after the introduction of methane on SnO2-based anodes. A measurable depolarization effect and lower consumption of carbon after the introduction of methane on carbon anodes were also demonstrated.

  19. A model for pore growth in anodically etched gallium phosphide

    NASA Astrophysics Data System (ADS)

    Ricci, P. C.; Salis, M.; Anedda, A.

    2005-06-01

    The electrochemical etching process of porous gallium phosphide was studied by means of the characteristic current-potential (I-V) curves. Measurements were performed in H2SO4 0.5-M aqueous solution both in the dark and by illuminating the samples with the 351-nm line of an argon laser. Raman spectroscopy was applied to investigate the surface morphology of the samples prepared under different anodizing conditions within the potentiostatic regime. Based on a few reasonable assumptions, a simple model of pore growth is proposed. The enhancing effect in current intensity due to the branching of pores and the opposite effect due to a concomitant decrease in the effective cross area available for carrier transport are accounted for to explain the main features of the recorded I -V curves.

  20. Current-limited imposed-potential technique for inducing and monitoring metastable pitting events

    SciTech Connect

    Wall, F.D.

    1999-11-24

    A technique has been developed to selectively induce metastable pitting while preventing the transition to stable pit growth. The current-limited imposed-potential (CLIP) technique limits available cathodic current to an initiated site using a resistor in series with the working electrode to form a voltage divider. Potentiodynamic CLIP testing yields a distribution of breakdown potentials from a single experiment. Potentiostatic CLIP testing yields induction time data, which can be used as input to a calculation of germination rate. Initial data indicate that a one-to-one correlation exists between electrochemical transients and observed pitting sites. The CLIP technique provides a consistent means of gathering quantitative potential and current transients associated with localized oxide breakdown.

  1. Preparation of Nickel Oxide Embedded Self Organized Titania Nanotubes Array by New Alginate Method as a Supercapacitor Electrode

    NASA Astrophysics Data System (ADS)

    Dabaghi, Habibeh Hadad; Kazemzad, Mahmood; Ganjkhanlou, Yadolah; Eskandari, Rahmatollah

    2013-12-01

    Potentiostatic two step anodizing of titanium utilized for preparation of self organized titania nanotubes arrays with diameter of 150 nm. Then the new alginate method has been applied for incorporation of NiO into the nanotubes. The prepared hybrid materials have been characterized by various methods including field emission scanning electron microscopy, X-ray diffractometry and cyclic voltammetry analyses. The X-ray diffraction patterns of samples were also studied by Rietveld's method. Results showed that the prepared electrode containing anatase, rutile and NiO phases with fraction of 70, 8, and 22%, respectively. It was found that by application of the new method, porous NiO uniformly coated on nanotubes surface and great enhancement of specific capacitance from 0.14 to 3.8 mF cm-2 could be obtained. The prepared nanocomposites are promising materials for supercapacitance application and also for solar energy harvesting systems.

  2. The relationship between induction time for pitting and pitting potential for high purity aluminum.

    SciTech Connect

    Wall, Frederick Douglas; Vandenavyle, Justin J.; Martinez, Michael A.

    2003-08-01

    The objective of this study was to determine if a distribution of pit induction times (from potentiostatic experiments) could be used to predict a distribution of pitting potentials (from potentiodynamic experiments) for high-purity aluminum. Pit induction times were measured for 99.99 Al in 50 mM NaCl at potentials of -0.35, -0.3, -0.25, and -0.2 V vs. saturated calomel electrode. Analysis of the data showed that the pit germination rate generally was an exponential function of the applied potential; however, a subset of the germination rate data appeared to be mostly potential insensitive. The germination rate behavior was used as an input into a mathematical relationship that provided a prediction of pitting potential distribution. Good general agreement was found between the predicted distribution and an experimentally determined pitting potential distribution, suggesting that the relationships presented here provide a suitable means for quantitatively describing pit germination rate.

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

    PubMed

    Gutirrez Pineda, Eduart; Alcaide, Francisco; Rodrguez Presa, Mara J; Bolzn, Agustn E; Gervasi, Claudio A

    2015-02-01

    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. PMID:25569325

  4. Efficient direct solar-to-hydrogen conversion by in situ interface transformation of a tandem structure

    PubMed Central

    May, Matthias M.; Lewerenz, Hans-Joachim; Lackner, David; Dimroth, Frank; Hannappel, Thomas

    2015-01-01

    Photosynthesis is nature's route to convert intermittent solar irradiation into storable energy, while its use for an industrial energy supply is impaired by low efficiency. Artificial photosynthesis provides a promising alternative for efficient robust carbon-neutral renewable energy generation. The approach of direct hydrogen generation by photoelectrochemical water splitting utilizes customized tandem absorber structures to mimic the Z-scheme of natural photosynthesis. Here a combined chemical surface transformation of a tandem structure and catalyst deposition at ambient temperature yields photocurrents approaching the theoretical limit of the absorber and results in a solar-to-hydrogen efficiency of 14%. The potentiostatically assisted photoelectrode efficiency is 17%. Present benchmarks for integrated systems are clearly exceeded. Details of the in situ interface transformation, the electronic improvement and chemical passivation are presented. The surface functionalization procedure is widely applicable and can be precisely controlled, allowing further developments of high-efficiency robust hydrogen generators. PMID:26369620

  5. A novel method for generating quantitative local electrochemical impedance spectroscopy

    SciTech Connect

    Lillard, R.S. ); Moran, P.J. ); Isaacs, H.S. )

    1992-04-01

    This paper reports on a local electrochemical impedance spectroscopy (LEIS) technique for mapping the ac impedance distribution, as a function of frequency, of an electrode. In LEIS, as in traditional ac impedance methods, a sinusoidal voltage perturbation between the working and reference electrode is maintained by driving an ac current between the working electrode and a distant counterelectrode with a potentiostat. Local ac impedances are then derived from the ratio of the applied ac voltage and the local ac solution current density. The local ac current density is obtained from potential difference measurements near the electrode surface using a probe consisting of two micro-electrodes. By measuring the ac potential difference between the micro-electrodes, and knowing their separation distance and the solution conductivity, the local ac solution current density is derived. The accuracy of the local ac impedance data generated with this technique was established by investigating two model systems.

  6. Motion-driven electrochromic reactions for self-powered smart window system.

    PubMed

    Yeh, Min-Hsin; Lin, Long; Yang, Po-Kang; Wang, Zhong Lin

    2015-05-26

    The self-powered system is a promising concept for wireless networks due to its independent and sustainable operations without an external power source. To realize this idea, the triboelectric nanogenerator (TENG) was recently invented, which can effectively convert ambient mechanical energy into electricity to power up portable electronics. In this work, a self-powered smart window system was realized through integrating an electrochromic device (ECD) with a transparent TENG driven by blowing wind and raindrops. Driven by the sustainable output of the TENG, the optical properties, especially the transmittance of the ECD, display reversible variations due to electrochemical redox reactions. The maximum transmittance change at 695 nm can be reached up to 32.4%, which is comparable to that operated by a conventional electrochemical potentiostat (32.6%). This research is a substantial advancement toward the practical application of nanogenerators and self-powered systems. PMID:25808880

  7. High frequency reference electrode

    DOEpatents

    Kronberg, J.W.

    1994-05-31

    A high frequency reference electrode for electrochemical experiments comprises a mercury-calomel or silver-silver chloride reference electrode with a layer of platinum around it and a layer of a chemically and electrically resistant material such as TEFLON around the platinum covering all but a small ring or halo' at the tip of the reference electrode, adjacent to the active portion of the reference electrode. The voltage output of the platinum layer, which serves as a redox electrode, and that of the reference electrode are coupled by a capacitor or a set of capacitors and the coupled output transmitted to a standard laboratory potentiostat. The platinum may be applied by thermal decomposition to the surface of the reference electrode. The electrode provides superior high-frequency response over conventional electrodes. 4 figs.

  8. A New PC and LabVIEW Package Based System for Electrochemical Investigations

    PubMed Central

    Stević, Zoran; Andjelković, Zoran; Antić, Dejan

    2008-01-01

    The paper describes a new PC and LabVIEW software package based system for electrochemical research. An overview of well known electrochemical methods, such as potential measurements, galvanostatic and potentiostatic method, cyclic voltammetry and EIS is given. Electrochemical impedance spectroscopy has been adapted for systems containing large capacitances. For signal generation and recording of the response of investigated electrochemical cell, a measurement and control system was developed, based on a PC P4. The rest of the hardware consists of a commercially available AD-DA converter and an external interface for analog signal processing. The interface is a result of authors own research. The software platform for desired measurement methods is LabVIEW 8.2 package, which is regarded as a high standard in the area of modern virtual instruments. The developed system was adjusted, tested and compared with commercially available system and ORCAD simulation.

  9. A straightforward implementation of in situ solution electrochemical C NMR spectroscopy for studying reactions on commercial electrocatalysts: ethanol oxidation.

    PubMed

    Huang, L; Sorte, E G; Sun, S-G; Tong, Y Y J

    2015-05-11

    Identifying and quantifying electrocatalytic-reaction-generated solution species, be they reaction intermediates or products, are highly desirable in terms of understanding the associated reaction mechanisms. We report herein a straightforward implementation of in situ solution electrochemical (13)C NMR spectroscopy for the first time that enables in situ studies of reactions on commercial fuel-cell electrocatalysts (Pt and PtRu blacks). Using ethanol oxidation reaction (EOR) as a working example, we discovered that (1) the complete oxidation of ethanol to CO2 only took place dominantly at the very beginning of a potentiostatic chronoamperometric (CA) measurement and (2) the PtRu had a much higher activity in catalysing oxygen insertion reaction that leads to acetic acid. PMID:25868425

  10. Corrosion behavior of sensitized duplex stainless steel.

    PubMed

    Torres, F J; Panyayong, W; Rogers, W; Velasquez-Plata, D; Oshida, Y; Moore, B K

    1998-01-01

    The present work investigates the corrosion behavior of 2205 duplex stainless steel in 0.9% NaCl solution after various heat-treatments, and compares it to that of 316L austenitic stainless steel. Both stainless steels were heat-treated at 500, 650, and 800 degrees C in air for 1 h, followed by furnace cooling. Each heat-treated sample was examined for their microstructures and Vickers micro-hardness, and subjected to the X-ray diffraction for the phase identification. Using potentiostatic polarization method, each heat-treated sample was corrosion-tested in 37 degrees C 0.9% NaCl solution to estimate its corrosion rate. It was found that simulated sensitization showed an adverse influence on both steels, indicating that corrosion rates increased by increasing the sensitization temperatures. PMID:9713683

  11. A new localized corrosion monitoring technique for the evaluation of oilfield inhibitors

    SciTech Connect

    Fu, S.L.; Griffin, A.M.; Garcia, J.G. Jr.

    1996-08-01

    Flow induced localized corrosion (FILC) is one of the major problems in the oilfield. Presently very few effective techniques are available for monitoring localized corrosion in oilfields. A new electrochemical technique was developed to provide a simple and effective way to monitor localized corrosion. The technique requires a potentiostat and a ZRA (zero resistance ammeter) as the measurement instrument. A special setup was designed to create a small anode and a large cathode. The technique was tested in a recirculating flow loop simulating FILC conditions. This technique was used to demonstrate the effectiveness of a corrosion inhibitor in mitigating localized corrosion. It can be further applied, both in the laboratory and in the field, to other areas where FILC is severe. 35 refs., 12 figs.

  12. Electrochemical deposition and characterization of Ni-P alloy thin films

    SciTech Connect

    Mahalingam, T. . E-mail: maha51@rediffmail.com; Raja, M.; Thanikaikarasan, S.; Sanjeeviraja, C.; Velumani, S.; Moon, Hosun; Kim, Yong Deak

    2007-08-15

    Nickel phosphorus (Ni-P) alloy thin films were prepared by electrodeposition on pre-cleaned copper substrates using a potentiostatic cathodic electrodeposition method from sulfate electrolyte baths at various sodium hypophosphite (NaH{sub 2}PO{sub 2}) concentrations. X-ray diffraction studies reveal polycrystalline cubic alloys at low concentrations of phosphorus (< 13.5 at.%) and these transformed into amorphous alloys at higher concentrations. X-ray photoelectron spectra show the presence of Ni{sub 2}p and P{sub 2}p lines corresponding to their binding energies. Scanning electron microscopic studies reveal spherical shaped grains at low phosphorus contents and modules of cauliflower type morphology at higher phosphorus concentrations. The effects of phosphorus concentration on the crystal structure, composition and morphology are studied and discussed.

  13. Photoelectrochemical effect on YBa/sub 2/Cu/sub 3/O/sub 7/ single crystals

    SciTech Connect

    Hampel, M.; Grabner, E.W.; Bachtler, M.; Lorenz, W.J.

    1989-02-01

    Electrochemical dc and transient measurements in the system YBa/sub 2/Cu/sub 3/O/sub 7// acetonitrile + tetrabutylammonium-perchlorate (as a supporting electrolyte) at T = 298 K showed a significant photoeffect on single crystal electrodes after irradiation with chopped white or monochromatic light under cathodic polarization conditions. The effect could not be observed on polycrystalline electrodes and on single crystals under anodic polarization conditions. Under potentiostatic control, the photoreduction current increased nearly exponentially with decreasing electrode potential. Obviously, an enhanced reduction of copper oxide components at the surface takes place during illumination. The photoeffect was found to depend on both the photon energy and the adjustment of the (twinned) single crystals and may be explained assuming a significant band gap in c-direction and an intrinsic photo-excitation of electrons from the valence band to the conduction band of the p-type conducting material.

  14. Electrochemical formation of Al-Tm intermetallics in eutectic LiCl-KCl melt containing Tm and Al ions

    NASA Astrophysics Data System (ADS)

    Li, Xing; Yan, Yong-De; Zhang, Mi-Lin; Tang, Hao; Ji, De-Bin; Han, Wei; Xue, Yun; Zhang, Zhi-Jian

    2014-09-01

    This work focuses on investigating the electrochemical formation of Al-Tm and Al-Li-Tm alloys in LiCl-KCl-AlCl3-Tm2O3 melt on both W and Al electrodes. Thermodynamic calculation and electrochemical behavior of LiCl-KCl melt containing both AlCl3 and Tm2O3 showed that AlCl3 can chlorinate Tm2O3 to release Tm(III) ions. Three kinds of Al-Tm intermetallics at about -1.26, -1.32 and -1.43 V were detected by means of various electrochemical measurement techniques, i.e. cyclic voltammetry, square wave voltammetry and open circuit chronopotentiometry. Potentiostatic and galvanostatic electrolysis were carried out on Al and W electrodes to prepare Al-Tm and Al-Li-Tm alloys, respectively. The composition of Al-Li-Tm alloys was analyzed by inductive coupled plasma atomic emission spectrometer (ICP-AES).

  15. Enhanced removal of 8-quinolinecarboxylic acid in an activated carbon cloth by electroadsorption in aqueous solution.

    PubMed

    López-Bernabeu, S; Ruiz-Rosas, R; Quijada, C; Montilla, F; Morallón, E

    2016-02-01

    The effect of the electrochemical treatment (potentiostatic treatment in a filter-press electrochemical cell) on the adsorption capacity of an activated carbon cloth (ACC) was analyzed in relation with the removal of 8-quinolinecarboxylic acid pollutant from water. The adsorption capacity of an ACC is quantitatively improved in the presence of an electric field (electroadsorption process) reaching values of 96% in comparison to 55% in absence of applied potential. In addition, the cathodic treatment results in higher removal efficiencies than the anodic treatment. The enhanced adsorption capacity has been proved to be irreversible, since the removed compound remains adsorbed after switching the applied potential. The kinetics of the adsorption processes is also improved by the presence of an applied potential. PMID:26433936

  16. The alkaline zinc electrode as a mixed potential system

    NASA Technical Reports Server (NTRS)

    Fielder, W. L.

    1979-01-01

    Cathodic and anodic processes for the alkaline zinc electrode in 0.01 molar zincate electrolyte (9 molar hydroxide) were investigated. Cyclic voltammograms and current-voltage curves were obtained by supplying pulses through a potentiostat to a zinc rotating disk electrode. The data are interpreted by treating the system as one with a mixed potential; the processes are termed The zincate and corrosion reactions. The relative proportions of the two processes vary with the supplied potential. For the cathodic region, the cathodic corrosion process predominates at higher potentials while both processes occur simultaneously at a lower potential (i.e., 50 mV). For the anodic region, the anodic zincate process predominates at higher potentials while the anodic corrosion process is dominant at lower potential (i.e., 50 mV) if H2 is present.

  17. Effect of growth potential on the electrodeposition of CIS thin films

    NASA Astrophysics Data System (ADS)

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

    2013-02-01

    Thin films of copper indium diselenide (CIS) were prepared in aqueous bath by low-cost potentiostatic electrodeposition technique onto Fluorine doped tin oxide substrates. The deposition potential was optimized using cyclic voltammetry study in a ternary Cu-In-Se system. The films were characterized systematically with the aid of UV-Vis spectroscopy, IV measurements, X-ray diffraction, Scanning electron microscopy and Energy dispersive X-ray analysis. CIS films deposited for different growth potential shows the tetragonal structure with (112) preferential orientation. Annealing of the films at temperature 400°C not only improves the crystallinity of layers, but it also increases the grain size, which is suitable for the development of high efficiency solar cells.

  18. 3D Printed Microfluidic Device with Integrated Biosensors for Online Analysis of Subcutaneous Human Microdialysate.

    PubMed

    Gowers, Sally A N; Curto, Vincenzo F; Seneci, Carlo A; Wang, Chu; Anastasova, Salzitsa; Vadgama, Pankaj; Yang, Guang-Zhong; Boutelle, Martyn G

    2015-08-01

    This work presents the design, fabrication, and characterization of a robust 3D printed microfluidic analysis system that integrates with FDA-approved clinical microdialysis probes for continuous monitoring of human tissue metabolite levels. The microfluidic device incorporates removable needle type integrated biosensors for glucose and lactate, which are optimized for high tissue concentrations, housed in novel 3D printed electrode holders. A soft compressible 3D printed elastomer at the base of the holder ensures a good seal with the microfluidic chip. Optimization of the channel size significantly improves the response time of the sensor. As a proof-of-concept study, our microfluidic device was coupled to lab-built wireless potentiostats and used to monitor real-time subcutaneous glucose and lactate levels in cyclists undergoing a training regime. PMID:26070023

  19. Reduction mechanism of sulfur in lithium-sulfur battery: From elemental sulfur to polysulfide

    NASA Astrophysics Data System (ADS)

    Zheng, Dong; Zhang, Xuran; Wang, Jiankun; Qu, Deyu; Yang, Xiaoqing; Qu, Deyang

    2016-01-01

    The polysulfide ions formed during the first reduction wave of sulfur in Li-S battery were determined through both in-situ and ex-situ derivatization of polysulfides. By comparing the cyclic voltammetric results with and without the derivatization reagent (methyl triflate) as well as the in-situ and ex-situ derivatization results under potentiostatic condition, in-situ derivatization was found to be more appropriate than its ex-situ counterpart, since subsequent fast chemical reactions between the polysulfides and sulfur may occur during the timeframe of ex-situ procedures. It was found that the major polysulfide ions formed at the first reduction wave of elemental sulfur were the S4 2 - and S5 2 - species, while the widely accepted reduction products of S8 2 - and S6 2 - for the first reduction wave were in low abundance.

  20. Effect of microstructure and strain on the degradation behavior of novel bioresorbable iron-manganese alloy implants.

    PubMed

    Heiden, Michael; Kustas, Andrew; Chaput, Kevin; Nauman, Eric; Johnson, David; Stanciu, Lia

    2015-02-01

    Advancing the understanding of microstructural effects and deformation on the degradability of Fe-Mn bioresorbable alloys (specifically, Fe-33%Mn) will help address the current problems associated with designing degradable fracture fixation implants for hard tissues. Potentiostatic polarization tests were conducted on a wide variety of metal samples to examine how different deformation processes affect the instantaneous rate of degradation of Fe-Mn alloys. Large-strain machining (LSM), a novel severe plastic deformation (SPD) technique was utilized during these experiments to modify the degradation properties of the proposed Fe-Mn alloy. It was discovered that Fe-33%Mn after LSM with a rake angle of 0° (effective strain = 2.85) showed the most promising increase in degradation rate compared to as-cast, annealed, and additional deformation conditions (rolled and other LSM parameters) for the same alloy. The mechanisms for enhancement of the corrosion rate are discussed. PMID:24825402

  1. Improvement of corrosion resistance of Nisbnd Mo alloy coatings: Effect of heat treatment

    NASA Astrophysics Data System (ADS)

    Mousavi, R.; Bahrololoom, M. E.; Deflorian, F.; Ecco, L.

    2016-02-01

    In this paper, Nisbnd Mo alloy coatings were deposited from bath containing sodium citrate, nickel sulphate, and sodium molybdate. Essentially, this work is divided into two mains parts: (i) the optimization on the coatings deposition parameters and (ii) the effect of the heat treatment. Polarization curves and electrochemical impedance spectroscopy were acquired using potentiostat/galvanostat and a frequency response analyzer, respectively. Morphology and chemical composition of the coatings were investigated by scanning electron microscopy and energy dispersive spectroscopy, respectively. Polarization curves at different condition revealed that electroplating at temperature 40 oC, pH 9 provides a dense coating with high efficiency. Following the optimization of the deposition parameters, the coatings were annealed at 200, 400, and 600 oC for 25 min. The results showed that the coatings obtained at temperature 40 oC, pH 9, and annealing at 600 oC has the highest corrosion resistance and microhardness.

  2. Efficient direct solar-to-hydrogen conversion by in situ interface transformation of a tandem structure

    NASA Astrophysics Data System (ADS)

    May, Matthias M.; Lewerenz, Hans-Joachim; Lackner, David; Dimroth, Frank; Hannappel, Thomas

    2015-09-01

    Photosynthesis is nature's route to convert intermittent solar irradiation into storable energy, while its use for an industrial energy supply is impaired by low efficiency. Artificial photosynthesis provides a promising alternative for efficient robust carbon-neutral renewable energy generation. The approach of direct hydrogen generation by photoelectrochemical water splitting utilizes customized tandem absorber structures to mimic the Z-scheme of natural photosynthesis. Here a combined chemical surface transformation of a tandem structure and catalyst deposition at ambient temperature yields photocurrents approaching the theoretical limit of the absorber and results in a solar-to-hydrogen efficiency of 14%. The potentiostatically assisted photoelectrode efficiency is 17%. Present benchmarks for integrated systems are clearly exceeded. Details of the in situ interface transformation, the electronic improvement and chemical passivation are presented. The surface functionalization procedure is widely applicable and can be precisely controlled, allowing further developments of high-efficiency robust hydrogen generators.

  3. Alkaline Ammonia Electrolysis on Electrodeposited Platinum for Controllable Hydrogen Production.

    PubMed

    Gwak, Jieun; Choun, Myounghoon; Lee, Jaeyoung

    2016-02-01

    Ammonia is beginning to attract a great deal of attention as an alternative energy source carrier, because clean hydrogen can be produced through electrolytic processes without the emission of COx . In this study, we deposited various shapes of Pt catalysts under potentiostatic mode; the electrocatalytic oxidation behavior of ammonia using these catalysts was studied in alkaline media. The electrodeposited Pt was characterized by both qualitative and quantitative analysis. To discover the optimal structure and the effect of ammonia concentration, the bulk pH value, reaction temperature, and applied current of ammonia oxidation were investigated using potential sweep and galvanostatic methods. Finally, ammonia electrolysis was conducted using a zero-gap cell, producing highly pure hydrogen with an energy efficiency over 80 %. PMID:26530809

  4. X-ray diffraction analysis of multilayer porous InP(001) structure

    SciTech Connect

    Lomov, A. A.; Punegov, V. I.; Vasil'ev, A. L.; Nohavica, D.; Gladkov, P.; Kartsev, A. A.; Novikov, D. V.

    2010-03-15

    Multilayer structures composed of four porous bilayers have been studied by high-resolution X-ray diffraction using synchrotron radiation, and the photoluminescence of these structures has been investigated at 4 K. The porous structures were formed by anodic oxidation of InP(001) substrates in aqueous HCl solution. The structural parameters of the sublayers were varied by changing the electrochemical etching mode (potentiostatic/galvanostatic). The X-ray scattering intensity maps near the InP 004 reflection are obtained. A model for scattering from such systems is proposed based on the statistical dynamical diffraction theory. Theoretical scattering maps have been fitted to the experimental ones. It is shown that a mathematical analysis of the scattering intensity maps makes it possible to determine the structural parameters of sublayers. The reconstructed parameters (thickness, strain, and porosity of sublayers and the shape and arrangement of pores) are in satisfactory agreement with the scanning electron microscopy data.

  5. Distribution of initial current between bare and filmed surfaces; What is being measured in a scratched electrode test

    SciTech Connect

    Wei, R.P.; Gao, M. . Dept. of Mechanical Engineering and Mechanics)

    1991-12-01

    The paper reports that, aid in understanding the contribution of the large filmed surface to the measured initial current transient in a scratched electrode test, an in situ fracture technique was used to determine the distribution of currents between the bare and filmed surfaces following the sudden introduction of the bare surface under potentiostatic control. Measurements were made on a 304 stainless steel in deaerated 3.5 percent NaCl solution at room temperature and showed strong influence of the filmed surface on the measured initial current transient. The result support the earlier conclusion that the bare-surface current densities and repassivation kinetics in the literature, based on scratched electrode measurements, are significantly overstated and need to be re-examined.

  6. Rapid identification of conditions causing intergranular corrosion or intergranular stress corrosion cracking in sensitized alloy 600

    SciTech Connect

    Woodward, J.

    1984-12-01

    In 1973, Seys and van Haute introduced a technique for measuring pitting potentials. They called this technique the Static Potential Band Method. A metal wire was mounted in a corrosion cell with counter and reference electrodes, and an electrical connection made to one end. A potential was applied with a potentiostat. At the same time, a constant current was passed through the wire to create a potential gradient in the metal phase; the result was the creation of a gradient in the electrode potential along the wire. This technique has many applications in corrosion studies. In this work, it has been applied to the intergranular corrosion (IGC) and intergranular stress corrosion cracking (IGSCC) of sensitized Alloy 600 in a sulfur-containing environment.

  7. 3D Printed Microfluidic Device with Integrated Biosensors for Online Analysis of Subcutaneous Human Microdialysate

    PubMed Central

    2015-01-01

    This work presents the design, fabrication, and characterization of a robust 3D printed microfluidic analysis system that integrates with FDA-approved clinical microdialysis probes for continuous monitoring of human tissue metabolite levels. The microfluidic device incorporates removable needle type integrated biosensors for glucose and lactate, which are optimized for high tissue concentrations, housed in novel 3D printed electrode holders. A soft compressible 3D printed elastomer at the base of the holder ensures a good seal with the microfluidic chip. Optimization of the channel size significantly improves the response time of the sensor. As a proof-of-concept study, our microfluidic device was coupled to lab-built wireless potentiostats and used to monitor real-time subcutaneous glucose and lactate levels in cyclists undergoing a training regime. PMID:26070023

  8. Investigation on the Oxidation and Reduction of Titanium in Molten Salt with the Soluble TiC Anode

    NASA Astrophysics Data System (ADS)

    Wang, Shulan; Wan, Chaopin; Liu, Xuan; Li, Li

    2015-12-01

    To reveal the oxidation process of titanium from TiC anode and the reduction mechanism of titanium ions in molten NaCl-KCl, the polarization curve of TiC anode in molten NaCl-KCl and cyclic voltammograms of the molten salt after polarization were studied. Investigation on the polarization curve shows that titanium can be oxidized and dissociated from the TiC anode at very low potential. The cyclic voltammograms demonstrated that the reduction reaction of titanium ions in the molten salt is a one-step process. By potentiostatic electrolysis, dendritic titanium is obtained on the steel plate. The work promotes the understanding on the process of electrochemical oxidization/dissociation of titanium from TiC anode and the reduction mechanism of titanium ions in molten salt.

  9. Structural and compositional characterization of Bi1-xSbx nanowire arrays grown by pulsed deposition to improve growth uniformity

    NASA Astrophysics Data System (ADS)

    Cassinelli, M.; Müller, S.; Aabdin, Z.; Peranio, N.; Eibl, O.; Trautmann, C.; Toimil-Molares, M. E.

    2015-12-01

    Arrays of Bi1-xSbx nanowire with various compositions (0 ⩽ x ⩽ 1) are grown in etched ion-track membranes by pulsed electrochemical deposition. Nanowires of diameter from 130 nm down to 18 nm are characterized by means of X-ray diffraction and high-resolution electron microscopy combined with electron diffraction and energy dispersive X-ray analysis. Compared to potentiostatic deposition, the pulsed synthesis method leads to a more uniform growth and higher filling rate of the wires across the entire template. By tuning the deposition parameters, we demonstrate excellent control over the wire composition and crystallographic orientation. The deposition process presented facilitates the development of future nanowire-based thermoelectric sensors, which are expected to exhibit a higher sensitivity and a faster response compared to thin film sensors.

  10. Corrosion behavior of boride layers evaluated by the EIS technique

    NASA Astrophysics Data System (ADS)

    Campos, I.; Palomar-Pardavé, M.; Amador, A.; VillaVelázquez, C.; Hadad, J.

    2007-09-01

    The corrosion behavior of boride layers at the AISI 304 steel surface is evaluated in the present study. Electrochemical impedance spectroscopy (EIS) technique was used for the evaluation of the polarization resistance at the steel surface, with the aid of AUTOLAB potentiostat. Samples were treated with boron paste thickness of 4 and 5 mm, in the range of temperatures 1123 ≤ T ≤ 1273 K and exposed time of 4 and 6 h. The electrochemical technique employed 10 mV AC with a frequency scan range from 8 kHz to 3 mHz in deaerated 0.1 M NaCl solution. Nyquist diagrams show that the highest values of corrosion resistance are present in the samples borided at the temperature of 1273 K, with treatment time of 4 h and 4 mm of boron paste thickness. The values of corrosion resistance on borided steels are compared with the porosity exhibited in the layers.

  11. Corrosion inhibition of mild steel in acidic media using newly synthesized heterocyclic organic molecules: Correlation between inhibition efficiency and chemical structure

    NASA Astrophysics Data System (ADS)

    Ouici, H. B.; Benali, O.; Guendouzi, A.

    2015-03-01

    The corrosion inhibition of mild steel in 5% HCl solutions by some new synthesized organic compounds namely 3-(2-methoxyphenyl) 5-mercapto-1. 2. 4-triazole (2-MMT), 3-(3-methoxyphenyl) 5-mercapto-1. 2. 4-triazole (3-MMT) and 3-(2-hydroxyphenyl) 5-mercapto-1. 2. 4-triazole (2-HMT) was investigated using weight loss and potentiostatic polarization techniques. These measurements reveal that the inhibition efficiency obtained by these compounds increased by increasing their concentration. The inhibition efficiency follows the order 2-MMT >3-MMT >2-HMT. Polarization studies show that these compounds are of the mixed type but dominantly act as a cathodic inhibitors for mild steel in 5% HCl solutions. These inhibitors function through adsorption following Langmuir isotherm. Activation energy and Gibbs free energy for adsorption of inhibitors are calculated. Molecular modeling has been conducted to correlate the corrosion inhibition properties with the calculated quantum chemical parameters.

  12. Electro-active sensor, method for constructing the same; apparatus and circuitry for detection of electro-active species

    NASA Technical Reports Server (NTRS)

    Buehler, Martin (Inventor)

    2009-01-01

    An electro-active sensor includes a nonconductive platform with a first electrode set attached with a first side of a nonconductive platform. The first electrode set serves as an electrochemical cell that may be utilized to detect electro-active species in solution. A plurality of electrode sets and a variety of additional electrochemical cells and sensors may be attached with the nonconductive platform. The present invention also includes a method for constructing the aforementioned electro-active sensor. Additionally, an apparatus for detection and observation is disclosed, where the apparatus includes a sealable chamber for insertion of a portion of an electro-active sensor. The apparatus allows for monitoring and detection activities. Allowing for control of attached cells and sensors, a dual-mode circuitry is also disclosed. The dual-mode circuitry includes a switch, allowing the circuitry to be switched from a potentiostat to a galvanostat mode.

  13. A one-compartment fructose/air biological fuel cell based on direct electron transfer.

    PubMed

    Wu, Xuee; Zhao, Feng; Varcoe, John R; Thumser, Alfred E; Avignone-Rossa, Claudio; Slade, Robert C T

    2009-10-15

    The construction and characterization of a one-compartment fructose/air biological fuel cell (BFC) based on direct electron transfer is reported. The BFC employs bilirubin oxidase and d-fructose dehydrogenase adsorbed on a cellulose-multiwall carbon nanotube (MWCNT) matrix, reconstituted with an ionic liquid, as the biocathode and the bioanode for oxygen reduction and fructose oxidation reactions, respectively. The performance of the bioelectrode was investigated by chronoamperometric and cyclic voltammetric techniques in a standard three-electrode cell, and the polarization and long-term stability of the BFC was tested by potentiostatic discharge. An open circuit voltage of 663 mV and a maximum power density of 126 microWcm(-2) were obtained in buffer at pH 5.0. Using this regenerated cellulose-MWCNT matrix as the immobilization platform, this BFC has shown a relatively high performance and long-term stability compared with previous studies. PMID:19674887

  14. Electrochemical flowcell for in-situ investigations by soft x-ray absorption and emission spectroscopy

    SciTech Connect

    Schwanke, C.; Lange, K. M.; Golnak, R.; Xiao, J.

    2014-10-15

    A new liquid flow-cell designed for electronic structure investigations at the liquid-solid interface by soft X-ray absorption and emission spectroscopy is presented. A thin membrane serves simultaneously as a substrate for the working electrode and solid state samples as well as for separating the liquid from the surrounding vacuum conditions. In combination with counter and reference electrodes this approach allows in-situ studies of electrochemical deposition processes and catalytic reactions at the liquid-solid interface in combination with potentiostatic measurements. As model system in-situ monitoring of the deposition process of Co metal from a 10 mM CoCl{sub 2} aqueous solution by X-ray absorption and emission spectroscopy is presented.

  15. Growth of expanded antimonial lead alloy battery grids

    SciTech Connect

    Tang, N.Y.; Valeriote, E.M.L.

    1995-07-01

    The creep strength of battery grids, expanded from drum-cast low-antimony lead alloy tip, wa varied by heat-treatments at several temperature. Grid growth following potentiostatic corrosion was found to be highly anisotropic. In spite of an increase in length, there wa a decrease in width. A theoretical analysis indicated that growth of expanded grids consisted of two components: an increase in the wire length (wire elongation), and a change in the grid shape (grid shear). The rate of the wire elongation is the corrosion test was found to be inversely related to the grid creep strength, and the deformation mechanism was identified as power-law creep. It is shown that, in order to meaningfully compare grid growths, the geometrical environment of grid test samples must be carefully controlled.

  16. Electrochemical generation of phosphorus-containing ion-radicals with simultaneous recording of EPR signal and electrochemical characteristics

    SciTech Connect

    Il'yasov, A.V.; Kadirov, M.K.; Kargin, Yu.M.

    1987-12-01

    The electrochemical generation of ion-radicals, especially under controlled conditions, widens the possibilities of a thorough theoretical analysis of the electronic structure of the compounds and of the rules governing the consecutive chemical reactions. In this work, the authors used a specially constructed three-electrode spiral vacuum cell to study at various temperatures certain unsaturated organophosphorus compounds containing two phosphorus atoms in the molecule. The possibility was envisaged of applying galvanometric pulses to the working electrode, containing the EPR spectrometer resonator, while controlling the potential, time, and intensity of the EPR signal, as well as poentiodynamic and potentiostatic pulses. The EPR spectra were recorded on a Bruker-Physik spectrometer. HFS constants are given for the ion-radicals studied.

  17. Efficient direct solar-to-hydrogen conversion by in situ interface transformation of a tandem structure.

    PubMed

    May, Matthias M; Lewerenz, Hans-Joachim; Lackner, David; Dimroth, Frank; Hannappel, Thomas

    2015-01-01

    Photosynthesis is nature's route to convert intermittent solar irradiation into storable energy, while its use for an industrial energy supply is impaired by low efficiency. Artificial photosynthesis provides a promising alternative for efficient robust carbon-neutral renewable energy generation. The approach of direct hydrogen generation by photoelectrochemical water splitting utilizes customized tandem absorber structures to mimic the Z-scheme of natural photosynthesis. Here a combined chemical surface transformation of a tandem structure and catalyst deposition at ambient temperature yields photocurrents approaching the theoretical limit of the absorber and results in a solar-to-hydrogen efficiency of 14%. The potentiostatically assisted photoelectrode efficiency is 17%. Present benchmarks for integrated systems are clearly exceeded. Details of the in situ interface transformation, the electronic improvement and chemical passivation are presented. The surface functionalization procedure is widely applicable and can be precisely controlled, allowing further developments of high-efficiency robust hydrogen generators. PMID:26369620

  18. Influence of surface modification of nitinol with silicon using plasma-immersion ion implantation on the alloy corrosion resistance in artificial physiological solutions

    NASA Astrophysics Data System (ADS)

    Kashin, O. A.; Borisov, D. P.; Lotkov, A. I.; Abramova, P. V.; Korshunov, A. V.

    2015-10-01

    Cyclic voltammetry and potentiostatic polarization have been applied to study electrochemical behavior and to determine corrosion resistance of nitinol, which surface was modified with silicon using plasma-immersion ion implantation, in 0.9% NaCl solution and in artificial blood plasma. It was found out that continuous, and also homogeneous in composition, thin Si-containing layers are resistant to corrosion damage at high positive potentials in artificial physiological solutions due to formation of stable passive films. Breakdown potential Eb of Si-modified NiTi depends on the character of silicon and Ni distribution at the alloy surface, Eb values amounted to 0.9-1.5 V (Ag/AgCl/KCl sat.) for the alloy samples with continuous Si-containing surface layers and with decreased Ni surface concentration.

  19. Improving the corrosion resistance of nitinol by plasma-immersion ion implantation with silicon for biomedical applications

    NASA Astrophysics Data System (ADS)

    Abramova, P. V.; Korshunov, A. V.; Lotkov, A. I.; Kashin, O. A.; Borisov, D. P.

    2015-11-01

    Cyclic voltammetry and potentiostatic polarization have been applied to study electrochemical behavior and to determine corrosion resistance of nitinol, which surface was modified with silicon using plasma-immersion ion implantation, in 0.9 % NaCl solution and in artificial blood plasma. It was found out that continuous, and also homogeneous in composition thin Si-containing layers are resistant to corrosion damage at high positive potentials in artificial physiological solutions due to formation of stable passive films. Breakdown potential Eb of Si-modified NiTi depends on the character of silicon and Ni distribution at the alloy surface, Eb values amounted to 0.9-1.5 V (Ag/AgCl/KCl sat.) for the alloy samples with continuous Si-containing surface layers and with decreased Ni surface concentration.

  20. Electrochemical durability of heat-treated carbon nanospheres as catalyst supports for proton exchange membrane fuel cells.

    PubMed

    Lv, Haifeng; Wu, Peng; Wan, Wei; Mu, Shichun

    2014-09-01

    Carbon nanospheres is wildly used to support noble metal nanocatalysts in proton exchange membrane (PEM) fuel cells, however they show a low resistance to electrochemical corrosion. In this study, the N-doped treatment of carbon nanospheres (Vulcan XC-72) is carried out in ammonia gas. The effect of heating treatment (up to 1000 degrees C) on resistances to electrochemical oxidation of the N-doped carbon nanospheres (HNC) is investigated. The resistance to electrochemical oxidation of carbon supports and stability of the catalysts are investigated with potentiostatic oxidation and accelerated durability test by simulating PEM fuel cell environment. The HNC exhibit a higher resistance to electrochemical oxidation than traditional Vulcan XC-72. The results show that the N-doped carbon nanospheres have a great potential application in PEM fuel cells. PMID:25924366

  1. Use of cyclic current reversal polarization voltammetry for investigating the relationship between corrosion resistance and heat-treatment induced variations in microstructures of 400 C martensitic stainless steels

    NASA Technical Reports Server (NTRS)

    Ambrose, John R.

    1992-01-01

    Software for running a cyclic current reversal polarization voltammagram has been developed for use with a EG&G Princeton Applied Research Model 273 potentiostat/galvanostat system. The program, which controls the magnitude, direction and duration of an impressed galvanostatic current, will produce data in ASCII spreadsheets (Lotus, Quattro) for graphical representation of CCRPV voltammograms. The program was used to determine differences in corrosion resistance of 440 C martenstic stainless steel produced as a result of changes in microstructure effected by tempering. It was determined that tempering at all temperatures above 400 F resulted in increased polarizability of the material, with the increased likelihood that pitting would be initiated upon exposure to marine environments. These results will be used in development of remedial procedures for lowering the susceptibility of these alloys toward the stress corrosion cracking experienced in bearings used in high pressure oxygen turbopumps used in the main engines of space shuttle orbiters.

  2. Polymer electrolyte fuel cell performance degradation at different synchrotron beam intensities.

    PubMed

    Eller, Jens; Bchi, Felix N

    2014-01-01

    The degradation of cell performance of polymer electrolyte fuel cells under monochromatic X-ray irradiation at 13.5?keV was studied in galvanostatic and potentiostatic operation modes in a through-plane imaging direction over a range of two orders of magnitude beam intensity at the TOMCAT beamline of the Swiss Light Source. The performance degradation was found to be a function of X-ray dose and independent of beam intensity, whereas the degradation rate correlates with beam intensity. The cell performance was more sensitive to X-ray irradiation at higher temperature and gas feed humidity. High-frequency resistance measurements and the analysis of product water allow conclusions to be drawn on the dominating degradation processes, namely change of hydrophobicity of the electrode and sulfate contamination of the electrocatalyst. PMID:24365920

  3. Use of array of conducting polymers for differentiation of coconut oil products.

    PubMed

    Rañola, Rey Alfred G; Santiago, Karen S; Sevilla, Fortunato B

    2016-01-01

    An array of chemiresistors based on conducting polymers was assembled for the differentiation of coconut oil products. The chemiresistor sensors were fabricated through the potentiostatic electrodeposition of polyaniline (PANi), polypyrrole (PPy) and poly(3-methylthiophene) (P-3MTp) on the gap separating two planar gold electrodes set on a Teflon substrate. The change in electrical resistance of the sensors was measured and observed after exposing the array to the headspace of oil samples. The sensor response was found rapid, reversible and reproducible. Different signals were obtained for each coconut oil sample and pattern recognition techniques were employed for the analysis of the data. The developed system was able to distinguish virgin coconut oil (VCO) from refined, bleached & deodorised coconut oil (RBDCO), flavoured VCO, homemade VCO, and rancid VCO. PMID:26695237

  4. Copper-selective electrochemical filling of macropore arrays for through-silicon via applications

    PubMed Central

    2012-01-01

    In this article, the physico-chemical and electrochemical conditions of through-silicon via formation were studied. First, macropore arrays were etched through a low doped n-type silicon wafer by anodization under illumination into a hydrofluoric acid-based electrolyte. After electrochemical etching, ‘almost’ through-silicon macropores were locally opened by a backside photolithographic process followed by anisotropic etching. The 450 × 450-μm² opened areas were then selectively filled with copper by a potentiostatic electrochemical deposition. Using this process, high density conductive via (4.5 × 105 cm−²) was carried out. The conductive paths were then electrically characterized, and a resistance equal to 32 mΩ/copper-filled macropore was determined. PMID:22776559

  5. Corrosion behavior of PIRAC nitrided Ti-6Al-4V surgical alloy.

    PubMed

    Starosvetsky, D; Shenhar, A; Gotman, I

    2001-02-01

    Hard titanium nitride (TiN) coatings were obtained on the surface of Ti-6Al-4V alloy using an original PIRAC nitriding method, based on annealing the samples under a low pressure of monatomic nitrogen created by selective diffusion of N from the atmosphere. PIRAC nitrided samples exhibited excellent corrosion resistance in Ringer's solution in both potentiodynamic and potentiostatic tests. The anodic current and metal ion release rate of PIRAC nitrided Ti-6Al-4V at the typical corrosion potential values were significantly lower than those of the untreated alloy. This, together with the excellent adhesion and high wear resistance of the TiN coatings, makes PIRAC nitriding an attractive surface treatment for Ti-6Al-4V alloy surgical implants. PMID:15348321

  6. Stationary anodic process at platinum in KF-NaF-AlF3-Al2O3 melts

    NASA Astrophysics Data System (ADS)

    Nekrasov, V. N.; Limanovskaya, O. V.; Suzdal'tsev, A. V.; Khramov, A. P.; Zaikov, Yu. P.

    2014-08-01

    The kinetics of the anodic process at platinum in KF-NaF-AlF3-Al2O3 melts in the temperature range 725-800°C is studied using potentiostatic polarization. Platinum is considered as an indifferent oxygen-evolving electrode, and a two-stage scheme is proposed for the anodic process on it. According to this scheme, primary charge transfer with the formation of adsorbed Oads particles is accompanied by their desorption according to a physical or an electrochemical mechanism. The polarization dependences of the anodic process on platinum are calculated under stationary conditions with allowance for the predominance of different stages of the process and a desorption mechanism. The calculated and experimental stationary anodic polarization dependences are compared.

  7. Inhibition of mild steel corrosion by sodium dodecyl benzene sulfonate and sodium oleate in acidic solutions

    SciTech Connect

    Luo, H.; Han, K.N.; Guan, Y.C.

    1998-08-01

    Inhibition of mild steel corrosion by sodium dodecyl benzene sulfonate (C{sub 12}H{sub 25}C{sub 6}H{sub 4}SO{sub 3}Na [SDBS]) and sodium oleate (CH{sub 3}[CH{sub 2}]{sub 7}CH{double_bond}CH[CH{sub 2}]{sub 7}COONa) in acidic solutions was investigated using a potentiostat, a lock-in amplifier, a contact angle goniometer, A fourier transform infrared (FTIR) spectrometer, and an ultraviolet (UV)/visible spectrophotometer. In the presence of the organic inhibitors, the corrosion rate was reduced significantly, Anionic SDBS was adsorbed on the positively charged mild steel surface through the electrostatic attraction. However, for sodium oleate, the soluble oleic acid (CH{sub 3}[CH{sub 2}]{sub 7}CH{double_bond}CH[CH]{sub 7}COOH) chemisorbed on the steel surface at the first stage. Then, insoluble colloid adsorbed on the chemisorbed surface through van der Waals forces.

  8. Electrochemical and surface studies of zinc in alkaline solutions containing organic corrosion inhibitors

    NASA Astrophysics Data System (ADS)

    Ein-Eli, Y.; Auinat, M.; Starosvetsky, D.

    The electrochemical behavior of zinc in strong alkaline solutions containing 8.5 M of potassium hydroxide (KOH) and polymeric organic inhibitors was evaluated. The concentrations of the organic inhibitors studies were in the range of 400-4000 ppm and included polyethylene glycol (PEG), with a molecular weight of 600, and polyoxyethylen alkyl phosphate ester acid form (GAFAC RA600). The electrochemical studies included anodic, cathodic, and linear polarization along with potentiostatic studies. It was found that the inhibition properties of PEG, in the strong alkaline solution, are by far much more efficient than the inhibition capability of GAFAC RA600. Surface analysis obtained with the use of high resolution scanning electron microscopy (HRSEM) revealed different morphology characteristic developed at the zinc surface in the presence of the two inhibitors. A methodology employing electrochemical tests is proposed to quickly and conveniently evaluate inhibitors for Zn in alkaline media.

  9. Influence of sodium salts of organic acids as additives on localized corrosion of aluminum and its alloys

    SciTech Connect

    Raspini, I.A. )

    1993-10-01

    Localized pitting is best described by a characteristic parameter called the pitting potential values (E[sub p]). Although E[sub p] is governed by a number of factors, including alloy composition, metallurgical history, and the corrosive environment, the strongest effect on E[sub p] is produced by certain additives that differ from the aggressive anion and exert a beneficial effect. These are referred to as inhibitors. Potentiokinetic and potentiostatic anodic polarization curves were obtained on aluminum (Al) and Al alloys in mixed solutions containing sodium chloride with sodium benzoate, sodium acetate, or thioglycolic acid as inhibitors. Immersion time at the rest potential and corrosion products accumulated in the pits influenced the inhibition efficiency. Reliability of the polarization method was discussed.

  10. A nanostructured copper telluride thin film grown at room temperature by an electrodeposition method

    NASA Astrophysics Data System (ADS)

    Dhasade, S. S.; Han, S. H.; Fulari, V. J.

    2012-09-01

    Copper telluride onion flower like microstructures, constructed by quantum dots with various diameters, were obtained by a potentiostatic electrodeposition method at room temperature. The structural, optical, surface morphology, compositional analysis and Raman spectra properties of the deposited films have been studied using X-ray diffraction, optical absorption with scanning electron microscopy, EDAX, and Raman spectroscopy. The electrolyte concentration and deposition time can be used to control the diameter of the electrodeposited quantum dots to within a range of 50-55 nm. The films are found to be stoichiometric in composition. The optical constants such as the optical band gap energy and the optical absorption spectra show significant variation in their values with a change in deposition time. Upon deposition time the band gap energy increased from a value of 2.74 to 2.89 eV.

  11. Engineering PQS Biosynthesis Pathway for Enhancement of Bioelectricity Production in Pseudomonas aeruginosa Microbial Fuel Cells

    PubMed Central

    Cao, Bin; Seviour, Thomas; Nesatyy, Victor J.; Marsili, Enrico; Kjelleberg, Staffan; Givskov, Michael; Tolker-Nielsen, Tim; Song, Hao; Loo, Joachim Say Chye; Yang, Liang

    2013-01-01

    The biosynthesis of the redox shuttle, phenazines, in Pseudomonas aeruginosa, an ubiquitous microorganism in wastewater microflora, is regulated by the 2-heptyl-3,4-dihydroxyquinoline (PQS) quorum-sensing system. However, PQS inhibits anaerobic growth of P. aeruginosa. We constructed a P. aeruginosa strain that produces higher concentrations of phenazines under anaerobic conditions by over-expressing the PqsE effector in a PQS negative ΔpqsC mutant. The engineered strain exhibited an improved electrical performance in microbial fuel cells (MFCs) and potentiostat-controlled electrochemical cells with an approximate five-fold increase of maximum current density relative to the parent strain. Electrochemical analysis showed that the current increase correlates with an over-synthesis of phenazines. These results therefore demonstrate that targeting microbial cell-to-cell communication by genetic engineering is a suitable technique to improve power output of bioelectrochemical systems. PMID:23700414

  12. Li Diffusion and High-Voltage Cycling Behavior of Thin-Film LiCoO2 Cathodes

    SciTech Connect

    Jang, Y.-I.

    2001-10-02

    Mass transport and thermodynamic properties of Li{sub x}CoO{sub 2} were studied by the potentiostatic intermittent titration technique (PITT) using solid-state thin-film batteries that provide a well-defined diffusion geometry. Both the chemical diffusion coefficient and the thermodynamic factor have minima at the phase boundaries of the Li/vacancy ordered phase ''Li{sub 0.5}CoO{sub 2}''. The self-diffusion coefficient of Li has a minimum at x = 0.5 associated with the Li/vacancy ordering. As the degree of ordering increases, the nonmonotonic variations become more pronounced when approaching x = 0.5 in Li{sub x}CoO{sub 2}. We also show that thin-film LiCoO{sub 2} cathodes having grains of sub-micrometer size combined with the Li upon electrolyte exhibit excellent capacity retention when charged up to 4.5 V.

  13. Electrochemical Water Oxidation of Ultrathin Cobalt Oxide-Based Catalyst Supported onto Aligned ZnO Nanorods.

    PubMed

    Koteeswara Reddy, Nandanapalli; Winkler, Stefanie; Koch, Norbert; Pinna, Nicola

    2016-02-10

    A stable and durable electrochemical water oxidation catalyst based on CoO functionalized ZnO nanorods (NRs) is introduced. ZnO NRs were grown on fluorine-doped tin oxide (FTO) by using a low-temperature chemical solution method and were functionalized with cobalt oxide by electrochemical deposition. The electrochemical water oxidation performance of cobalt oxide functionalized ZnO NRs was studied under alkaline (pH = 10) conditions. From these studies, it is noticed that cobalt oxide functionalized ZnO NRs show electrocatalytic activity toward water oxidation with current density on the order of several mA cm(-2). Further, 30 s CoO deposited ZnO nanorods exhibited excellent galvanostatic stability at a current density of 1 mA cm(-2) and potentiostatic stability at 1.25 V vs Ag/AgCl over an electrolysis period of 1 h. PMID:26784675

  14. Light addressable potentiometric sensor with an array of sensing regions

    NASA Astrophysics Data System (ADS)

    Liang, Weiguo; Han, JingHong; Zhang, Hong; Chen, Deyong

    2001-09-01

    This paper describes the mechanism of light addressable poteniometric sensors (LAPS) from the viewpoints of Semiconductor Physics, and introduces the fabrication of a multi-parameter LAPS chip. The MEMS technology is applied to produce a matrix of sensing regions on the wafer. By doing that, the cross talk among these regions is reduced, and the precision of the LAPS is increased. An IR-LED matrix is used as the light source, and the flow-injection method is used to input samples. The sensor system is compact and highly integrated. The measure and control system is composed of a personal computer, a lock-in amplifier, a potentiostat, a singlechip system, and an addressing circuit. Some experiments have been done with this device. The results show that this device is very promising for practical use.

  15. High frequency reference electrode

    DOEpatents

    Kronberg, James W.

    1994-01-01

    A high frequency reference electrode for electrochemical experiments comprises a mercury-calomel or silver-silver chloride reference electrode with a layer of platinum around it and a layer of a chemically and electrically resistant material such as TEFLON around the platinum covering all but a small ring or "halo" at the tip of the reference electrode, adjacent to the active portion of the reference electrode. The voltage output of the platinum layer, which serves as a redox electrode, and that of the reference electrode are coupled by a capacitor or a set of capacitors and the coupled output transmitted to a standard laboratory potentiostat. The platinum may be applied by thermal decomposition to the surface of the reference electrode. The electrode provides superior high-frequency response over conventional electrodes.

  16. Standing and propagating wave oscillations in the anodic dissolution of nickle

    NASA Astrophysics Data System (ADS)

    Lev, O.; Sheintuch, M.; Pisemen, L. M.; Yarnitzkyt, Ch.

    1988-12-01

    Spontaneous pattern formation in reactive media has been thoroughly investigated in homogeneous oscillatory systems, mainly in the Belousov-Zhabotinsky reaction1. Spatiotemporal patterns have been observed in some studies of catalytic surfaces2,3 and of travelling electrochemical waves4. Here we report on oscilla-tory wave patterns observed during electrochemical dissolution of a nickel wire in acidic media. We show that space-averaged poten-tial or current oscillations are associated with the creation of an inhomogeneous current distribution, and that the selection of a specific spatial current pattern depends on the current control mode of the electrochemical cell. In the almost potentiostatic (fixed potential) mode of operation, a train of travelling pulses prevails, whereas antiphase oscillations occur in the galvanostatic (constant average current) mode. The latter, as far as we know, have never before been reported in any reactive system.

  17. Relation between energetic and utilization coefficients in the positive plates of automotive lead/acid batteries

    NASA Astrophysics Data System (ADS)

    D'Alkaine, C. V.; Carubelli, A.; Fava, H. W.; Sanhueza, A. C.

    A new experimental method to distinguish between energetic and structural materials and to characterize the manufacturing technology for positive plates in lead/acid batteries is discussed. This new method proposes the evaluation of the energetic β-coefficient from plots of capacity versus very low current densities under galvanostatic conditions and using real-size positive plates in 2.3-6.9 M H 2SO 4 solutions. The results are identical to those obtained previously from potentiostatic measurements, and they fit a new equation as opposed to Peukert's equation. The independence of the β-coefficient with H 2SO 4 concentration indicates that the discharge of PbO 2 to its products proceeds via a solid-state reaction mechanism.

  18. Surface enhanced Raman scattering of a lipid Langmuir monolayer at the air-water interface.

    PubMed

    Mangeney, C; Dupres, V; Roche, Y; Felidj, N; Levi, G; Aubard, J; Bernard, S

    Surface enhanced Raman spectra were recorded from a phospholipid monolayer directly at the air-water interface. We used an organized monolayer of negatively charged tetramyristoyl cardiolipins as a template for the electrochemical generation of silver deposits. This two-dimensional electrodeposition of silver under potentiostatic control was the substrate for enhancement of Raman spectra. We report the optimized conditions for the Raman enhancement, the microscopic observations of the deposits, and their characterization by atomic force microscopy. Laser excitation at 514.5 nm leads to intense and reproducible surface enhanced Raman scattering spectra recorded in situ from one monolayer of cardiolipin, using 0.5 mol % of 10N nonyl acridine orange or 5 mol % of acridine in the film, and demonstrates the possibility of estimating the pH at the metal/phospholipidic film interface. PMID:15137111

  19. Large-diameter titanium dioxide nanotube arrays as a scattering layer for high-efficiency dye-sensitized solar cell.

    PubMed

    Liu, Xiaolin; Guo, Min; Cao, Jianjun; Lin, Jia; Tsang, Yuen Hong; Chen, Xianfeng; Huang, Haitao

    2014-01-01

    Large-sized titanium dioxide (TiO2) nanotube arrays with an outer diameter of approximately 500 nm have been successfully synthesized by potentiostatic anodization at 180 V in a used electrolyte with the addition of 1.5 M lactic acid. It is found that the synthesized large-diameter TiO2 nanotube array shows a superior light scattering ability, which can be used as a light scattering layer to significantly enhance the efficiency of TiO2 nanoparticle-based dye-sensitized solar cells from 5.18% to 6.15%. The remarkable light scattering ability makes the large-diameter TiO2 nanotube array a promising candidate for light management in dye-sensitized solar cells (DSSCs). PMID:25114652

  20. Large-diameter titanium dioxide nanotube arrays as a scattering layer for high-efficiency dye-sensitized solar cell

    PubMed Central

    2014-01-01

    Large-sized titanium dioxide (TiO2) nanotube arrays with an outer diameter of approximately 500 nm have been successfully synthesized by potentiostatic anodization at 180 V in a used electrolyte with the addition of 1.5 M lactic acid. It is found that the synthesized large-diameter TiO2 nanotube array shows a superior light scattering ability, which can be used as a light scattering layer to significantly enhance the efficiency of TiO2 nanoparticle-based dye-sensitized solar cells from 5.18% to 6.15%. The remarkable light scattering ability makes the large-diameter TiO2 nanotube array a promising candidate for light management in dye-sensitized solar cells (DSSCs). PMID:25114652

  1. Corrosion inhibition of mild steel in acidic media using newly synthesized heterocyclic organic molecules: Correlation between inhibition efficiency and chemical structure

    SciTech Connect

    Ouici, H. B. Guendouzi, A.; Benali, O.

    2015-03-30

    The corrosion inhibition of mild steel in 5% HCl solutions by some new synthesized organic compounds namely 3-(2-methoxyphenyl) 5-mercapto-1. 2. 4-triazole (2-MMT), 3-(3-methoxyphenyl) 5-mercapto-1. 2. 4-triazole (3-MMT) and 3-(2-hydroxyphenyl) 5-mercapto-1. 2. 4-triazole (2-HMT) was investigated using weight loss and potentiostatic polarization techniques. These measurements reveal that the inhibition efficiency obtained by these compounds increased by increasing their concentration. The inhibition efficiency follows the order 2-MMT >3-MMT >2-HMT. Polarization studies show that these compounds are of the mixed type but dominantly act as a cathodic inhibitors for mild steel in 5% HCl solutions. These inhibitors function through adsorption following Langmuir isotherm. Activation energy and Gibbs free energy for adsorption of inhibitors are calculated. Molecular modeling has been conducted to correlate the corrosion inhibition properties with the calculated quantum chemical parameters.

  2. Electrochemical Polishing Applications and EIS of a Novel Choline Chloride-Based Ionic Liquid

    SciTech Connect

    Wixtrom, Alex I.; Buhler, Jessica E.; Reece, Charles E.; Abdel-Fattah, Tarek M.

    2013-06-01

    Minimal surface roughness is a critical feature for high-field superconducting radio frequency (SRF) cavities used to engineer particle accelerators. Current methods for polishing Niobium cavities typically utilize solutions containing a mixture of concentrated sulfuric and hydrofluoric acid. Polishing processes such as these are effective, yet there are many hazards and costs associated with the use (and safe disposal) of the concentrated acid solutions. An alternative method for electrochemical polishing of the cavities was explored using a novel ionic liquid solution containing choline chloride. Potentiostatic electrochemical impedance spectroscopy (EIS) was used to analyze the ionic polishing solution. Final surface roughness of the Nb was found to be comparable to that of the acid-polishing method, as assessed by atomic force microscopy (AFM). This indicates that ionic liquid-based electrochemical polishing of Nb is a viable replacement for acid-based methods for preparation of SRF cavities.

  3. Electron transfer mechanism in Shewanella loihica PV-4 biofilms formed at graphite electrode.

    PubMed

    Jain, Anand; Zhang, Xiaoming; Pastorella, Gabriele; Connolly, Jack O; Barry, Niamh; Woolley, Robert; Krishnamurthy, Satheesh; Marsili, Enrico

    2012-10-01

    Electron transfer mechanisms in Shewanella loihica PV-4 viable biofilms formed at graphite electrodes were investigated in potentiostat-controlled electrochemical cells poised at oxidative potentials (0.2V vs. Ag/AgCl). Chronoamperometry (CA) showed a repeatable biofilm growth of S. loihica PV-4 on graphite electrode. CA, cyclic voltammetry (CV) and its first derivative shows that both direct electron transfer (DET) mediated electron transfer (MET) mechanism contributes to the overall anodic (oxidation) current. The maximum anodic current density recorded on graphite was 90 μA cm(-2). Fluorescence emission spectra shows increased concentration of quinone derivatives and riboflavin in the cell-free supernatant as the biofilm grows. Differential pulse voltammetry (DPV) show accumulation of riboflavin at the graphite interface, with the increase in incubation period. This is the first study to observe a gradual shift from DET to MET mechanism in viable S. loihica PV-4 biofilms. PMID:22281091

  4. New Cyclic Voltammetry Method for Examining Phase Transitions on Electrodes: Simulated Results

    NASA Astrophysics Data System (ADS)

    Abou Hamad, Ibrahim; Robb, Daniel; Rikvold, Per Arne

    2007-03-01

    We propose a new experimental technique for cyclic voltammetry, based on the first-order reversal curve (FORC) method for analysis of systems undergoing hysteresis. The advantages of this technique are demonstrated by applying it to dynamical models of electrochemical adsorption. The method can not only differentiate between discontinuous and continuous phase transitions, but can also quite accurately recover equilibrium behavior from dynamic analysis of systems with a continuous phase transition. The FORC diagram for a discontinuous phase transition is characterized by a negative (unstable) region separating two positive (stable) regions, while such a negative region does not exist for continuous phase transitions. Experimental data for Electrochemical FORC (EC-FORC) analysis could easily be obtained by simple reprogramming of a potentiostat designed for conventional cyclic-voltammetry experiments.I. Abou Hamad, D.T. Robb, P.A. Rikvold, J. Electroanal. Chem., in press.

  5. Scanning droplet cell for high throughput electrochemical and photoelectrochemical measurements

    NASA Astrophysics Data System (ADS)

    Gregoire, John M.; Xiang, Chengxiang; Liu, Xiaonao; Marcin, Martin; Jin, Jian

    2013-02-01

    High throughput electrochemical techniques are widely applied in material discovery and optimization. For many applications, the most desirable electrochemical characterization requires a three-electrode cell under potentiostat control. In high throughput screening, a material library is explored by either employing an array of such cells, or rastering a single cell over the library. To attain this latter capability with unprecedented throughput, we have developed a highly integrated, compact scanning droplet cell that is optimized for rapid electrochemical and photoeletrochemical measurements. Using this cell, we screened a quaternary oxide library as (photo)electrocatalysts for the oxygen evolution (water splitting) reaction. High quality electrochemical measurements were carried out and key electrocatalytic properties were identified for each of 5456 samples with a throughput of 4 s per sample.

  6. Lab-on-a-chip sensor for measuring Zn by stripping voltammetry

    NASA Astrophysics Data System (ADS)

    Pei, Xing; Kang, Wenjing; Yue, Wei; Bange, Adam; Wong, Hector R.; Heineman, William R.; Papautsky, Ian

    2012-03-01

    This work reports on continuing development of a lab-on-a-chip sensor for electrochemical detection of heavy metal zinc in blood serum. The sensor consists of a three electrode system, including an environmentally-friendly bismuth working electrode, a Ag/AgCl reference electrode, and a gold auxiliary electrode. By optimizing the electrodeposition of bismuth film, better control of fabrication steps and improving interface between the sensor and potentiostat, repeatability and sensitivity of the lab-on-a-chip sensor has been improved. Through optimization of electrolyte and stripping voltammetry parameters, limits of detection were greatly improved. The optimized sensor was able to measure zinc in in the physiological range of 65-95 μg/dL. Ultimately, with further development and integrated sample preparation sensor system will permit rapid (min) measurements of zinc from a sub-mL sample (a few drops of blood) for bedside monitoring.

  7. Electro-Mechanical Actuation of Carbon Nanotube Yarns, Sheets, Composites

    NASA Astrophysics Data System (ADS)

    Oh, Jiyoung; Kozlov, Mikhail; Zhang, Mei; Fang, Shaoli; Baughman, Ray

    2011-03-01

    We report preparation of highly conductive carbon nanotube yarns and sheets. The materials aim at such applications as electronic textiles, electro-mechanical actuators, and conductive coatings. The electro-mechanical response of the specimens was measured using custom made force transducer operating in an isometric mode. The measurements were carried out at room temperature in aqueous and organic electrolytes; square-wave potential of variable amplitude was applied with a potentiostat. It was found that the maximum isometric stress generated by nanotube actuators could be as large as 12 MPa. This approaches the stress generation capability of commercial ferroelectrics and is significantly larger than that of natural muscles. A variety of applications of the materials is discussed.

  8. Electrochemical velocimetry on centrifugal microfluidic platforms.

    PubMed

    Abi-Samra, Kameel; Kim, Tae-Hyeong; Park, Dong-Kyu; Kim, Nahui; Kim, Jintae; Kim, Hanshin; Cho, Yoon-Kyoung; Madou, Marc

    2013-08-21

    Expanding upon recent applications of interfacing electricity with centrifugal microfluidic platforms, we introduce electrochemical velocimetry to monitor flow in real-time on rotating fluidic devices. Monitoring flow by electrochemical techniques requires a simple, compact setup of miniaturized electrodes that are embedded within a microfluidic channel and are connected to a peripherally-located potentiostat. On-disc flow rates, determined by electrochemical velocimetry, agreed well with theoretically expected values and with optical measurements. As an application of the presented techniques, the dynamic process of droplet formation and release was recorded, yielding critical information about droplet frequency and volume. Overall, the techniques presented in this work advance the field of centrifugal microfluidics by offering a powerful tool, previously unavailable, to monitor flow in real-time on rotating microfluidic systems. PMID:23787459

  9. Engineering PQS biosynthesis pathway for enhancement of bioelectricity production in pseudomonas aeruginosa microbial fuel cells.

    PubMed

    Wang, Victor Bochuan; Chua, Song-Lin; Cao, Bin; Seviour, Thomas; Nesatyy, Victor J; Marsili, Enrico; Kjelleberg, Staffan; Givskov, Michael; Tolker-Nielsen, Tim; Song, Hao; Loo, Joachim Say Chye; Yang, Liang

    2013-01-01

    The biosynthesis of the redox shuttle, phenazines, in Pseudomonas aeruginosa, an ubiquitous microorganism in wastewater microflora, is regulated by the 2-heptyl-3,4-dihydroxyquinoline (PQS) quorum-sensing system. However, PQS inhibits anaerobic growth of P. aeruginosa. We constructed a P. aeruginosa strain that produces higher concentrations of phenazines under anaerobic conditions by over-expressing the PqsE effector in a PQS negative ΔpqsC mutant. The engineered strain exhibited an improved electrical performance in microbial fuel cells (MFCs) and potentiostat-controlled electrochemical cells with an approximate five-fold increase of maximum current density relative to the parent strain. Electrochemical analysis showed that the current increase correlates with an over-synthesis of phenazines. These results therefore demonstrate that targeting microbial cell-to-cell communication by genetic engineering is a suitable technique to improve power output of bioelectrochemical systems. PMID:23700414

  10. Spectroscopic investigation of an electrochemically controlled conducting polymer-solid electrolyte junction

    NASA Astrophysics Data System (ADS)

    Berzina, Tatiana; Erokhin, Victor; Fontana, M. P.

    2007-01-01

    We have recently reported a hybrid conducting polymer-solid electrolyte heterojunction in which electronic channel current is controlled by ionic diffusion and redox reactions involving doped polyethyleneoxide and doped polyaniline (PANI). In this paper we demonstrate on the microscopic level the validity of the model we proposed to interpret the electronic behavior of the device we fabricated. In particular, we used resonance and vicinity (surface-enhanced-Raman-scattering like) enhanced micro-Raman spectroscopy to map out the redox state of PANI along the conducting channel, simultaneously with the determination of the voltamperometric characteristics in a potentiostat configuration. The Raman data were complemented as appropriate by the optical and Fourier transform infrared absorption spectroscopies.

  11. Surface phenomena of hydroxyapatite film on the nanopore formed Ti-29Nb-xZr alloy by anodization for bioimplants.

    PubMed

    Kim, Eun-Ju; Jeong, Yong-Hoon; Choe, Han-Cheol

    2013-03-01

    In this study, surface phenomena of hydroxyapatite (HA) film on the nanopore formed Ti-29Nb-xZr alloy by anodization for bioimplants have been investigated by electron beam physical vapor deposition (EB-PVD), field emission scanning electron microscope (FE-SEM), X-ray diffractometer (XRD), potentiostat and contact angle. The microstructure of Ti-29Nb-xZr alloys exhibited equiaxed structure and alpha" phase decreased, whereas beta phase increased as Zr content increased. The increment of Zr contents in HA coated nanotubular Ti-29Nb-xZr alloys showed good corrosion potential in 0.9% NaCI solution. The wettability of HA coated nanotubular surface was higher than that of non-coated samples. PMID:23755573

  12. First-Principles Molecular Dynamics at a Constant Electrode Potential

    NASA Astrophysics Data System (ADS)

    Bonnet, Nicéphore; Morishita, Tetsuya; Sugino, Osamu; Otani, Minoru

    2012-12-01

    A simulation scheme for performing first-principles molecular dynamics at a constant electrode potential is presented, opening the way for a more realistic modeling of voltage-driven devices. The system is allowed to exchange electrons with a reservoir at fixed potential, and dynamical equations for the total electronic charge are derived by using the potential energy of the extended system. In combination with a thermostat, this potentiostat scheme reproduces thermal fluctuations of the charge with the correct statistics, implying a realistic treatment of the potential as a control variable. Practically, the dynamics of the charge are decoupled from the electronic structure calculations, making the scheme easily implementable in existing first-principles molecular dynamics codes. Our approach is demonstrated on a test system by considering various test cases.

  13. Improving the signal-to-noise ratio of an ECL-based sensor using ad hoc carbon nanotube electrodes

    NASA Astrophysics Data System (ADS)

    Sanginario, A.; Giorcelli, M.; Tagliaferro, A.; Demarchi, D.

    2012-07-01

    In this paper, we demonstrate that mechanically modified cylinder-shaped carbon nanotube (CNT) working electrodes (WEs), combined with an averaging processing algorithm, can increase electrogenerated chemiluminescence (ECL) limit of detection by more than one order of magnitude, compared to gold electrodes. With CNT WEs, we obtained a stable light emission that lasts for hundreds of voltammetric cycles. This stability was further exploited to increase the detection limit with a simple algorithm, based on mean calculation. Ad hoc fabricated sensors are characterized with a full-custom potentiostat testbed and software platform, using tris(2,2-bipyridyl)ruthenium (II) as ECL labels. Our measurement results show that the signal-to-noise ratio (SNR) improves by a factor of larger than 20 compared to standard gold WEs to reach a detection limit up to 40 pg μl-1.

  14. A Complementary Type of Electrochromic Device by Radio Frequency Magnetron Sputtering System

    NASA Astrophysics Data System (ADS)

    Oksuz, Lutfi; Kiristi, Melek; Bozduman, Ferhat; Uygun Oksuz, Aysegul

    2014-10-01

    Electrochromic (EC) devices can change their optical properties reversibly in the visible region (400-800 nm) upon charge insertion/extraction reactions according to the applied voltage. A complementary type of EC device composes of two electrochromic layers, which is separated by an ionic conduction layer (electrolyte). In this work, the EC device was fabricated using vanadium oxide (V2O5) and titanium doped tungsten oxide (WO3-TiO2) electrodes. The EC electrodes were deposited as thin film structures by a reactive RF magnetron sputtering system in a medium of gas mixture of argon and oxygen. surface morphology of the films was characterized by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Electrochemical property and durability of the EC device was investigated by a potentiostat system. Optical measurement was examined under applied voltages of +/- 2.5 V by a computer-controlled system, constantly.

  15. First-principles molecular dynamics at a constant electrode potential.

    PubMed

    Bonnet, Nicéphore; Morishita, Tetsuya; Sugino, Osamu; Otani, Minoru

    2012-12-28

    A simulation scheme for performing first-principles molecular dynamics at a constant electrode potential is presented, opening the way for a more realistic modeling of voltage-driven devices. The system is allowed to exchange electrons with a reservoir at fixed potential, and dynamical equations for the total electronic charge are derived by using the potential energy of the extended system. In combination with a thermostat, this potentiostat scheme reproduces thermal fluctuations of the charge with the correct statistics, implying a realistic treatment of the potential as a control variable. Practically, the dynamics of the charge are decoupled from the electronic structure calculations, making the scheme easily implementable in existing first-principles molecular dynamics codes. Our approach is demonstrated on a test system by considering various test cases. PMID:23368585

  16. On-site fuel electroanalysis: determination of lead, copper and mercury in fuel bioethanol by anodic stripping voltammetry using screen-printed gold electrodes.

    PubMed

    Almeida, Eduardo S; Richter, Eduardo M; Munoz, Rodrigo A A

    2014-07-21

    The potential application of commercial screen-printed gold electrodes (SPGEs) for the trace determination of lead, copper, and mercury in fuel bioethanol is demonstrated. Samples were simply diluted in 0.067 mol L(-1) HCl solution prior to square-wave anodic stripping voltammetry (SWASV) measurements recorded with a portable potentiostat. The proposed method presented a low detection limit (<2 μg L(-1)) for a 240 s deposition time, linear range between 5 and 300 μg L(-1), and adequate recovery values (96-104%) for spiked samples. This analytical method shows great promise for on-site trace metal determination in fuel bioethanol once there is no requirement for sample treatment or electrode modification. PMID:25000856

  17. A high precision CMOS weak current readout circuit

    NASA Astrophysics Data System (ADS)

    Qisong, Wu; Haigang, Yang; Tao, Yin; Chong, Zhang

    2009-07-01

    This paper presents a high precision CMOS weak current readout circuit. This circuit is capable of converting a weak current into a frequency signal for amperometric measurements with high precision and further delivering a 10-bit digital output. A fast stabilization-enhanced potentiostat has been proposed in the design, which is used to maintain a constant bias potential for amperometric biochemical sensors. A technique based on source voltage shifting that reduces the leakage current of the MOS transistor to the reverse diode leakage level at room temperature was employed in the circuit. The chip was fabricated in the 0.35 μm chartered CMOS process, with a single 3.3 V power supply. The interface circuit maintains a dynamic range of more than 100 dB. Currents from 1 pA to 300 nA can be detected with a maximum nonlinearity of 0.3% over the full scale.

  18. Novel integrated and portable endotoxin detection system based on an electrochemical biosensor.

    PubMed

    Zuzuarregui, Ana; Souto, David; Pérez-Lorenzo, Eva; Arizti, Fernando; Sánchez-Gómez, Susana; Martínez de Tejada, Guillermo; Brandenburg, Klaus; Arana, Sergio; Mujika, Maite

    2015-01-21

    This paper describes the design, implementation and validation of a sensitive and integral technology solution for endotoxin detection. The unified and portable platform is based on the electrochemical detection of endotoxins using a synthetic peptide immobilized on a thin-film biosensor. The work covers the fabrication of an optimized sensor, the biofunctionalization protocol and the design and implementation of the measuring and signalling elements (a microfluidic chamber and a portable potentiostat-galvanostat), framed ad hoc for this specific application. The use of thin-film technologies to fabricate the biosensing device and the application of simple immobilization and detection methods enable a rapid, easy and sensitive technique for in situ and real time LPS detection. PMID:25431806

  19. Combinatorial electrochemical synthesis and screening of Pt-WO3 catalysts for electro-oxidation of methanol

    NASA Astrophysics Data System (ADS)

    Jayaraman, Shrisudersan; Baeck, Sung-Hyeon; Jaramillo, Thomas F.; Kleiman-Shwarsctein, Alan; McFarland, Eric W.

    2005-06-01

    An automated system for high-throughput electrochemical synthesis and screening of fuel cell electro-oxidation catalysts is described. This system consists of an electrode probe that contains counter and reference electrodes that can be positioned inside an array of electrochemical cells created within a polypropylene block. The electrode probe is attached to an automated of X-Y-Z motion system. An externally controlled potentiostat is used to apply the electrochemical potential to the catalyst substrate. The motion and electrochemical control are integrated using a user-friendly software interface. During automated synthesis the deposition potential and/or current may be controlled by a pulse program triggered by the software using a data acquisition board. The screening includes automated experiments to obtain cyclic voltammograms. As an example, a platinum-tungsten oxide (Pt-WO3) library was synthesized and characterized for reactivity towards methanol electro-oxidation.

  20. In vitro biocompatibility response of Ti-Zr-Si thin film metallic glasses

    NASA Astrophysics Data System (ADS)

    Ke, J. L.; Huang, C. H.; Chen, Y. H.; Tsai, W. Y.; Wei, T. Y.; Huang, J. C.

    2014-12-01

    In this study, the bio-electrochemical response of the Ti-Zr-Si thin film metallic glasses (TFMGs) in simulated body fluid with different contents of titanium is measured via potentiostat. According to the results of bio-corrosion potential and current, as well as the polarization resistance, it is concluded that the Ti66Zr25Si9 TFMGs possess the highest bio-electrochemical resistance. With increasing content of titanium, the corrosion resistance becomes progressively higher. The passive current results reveal that amorphous alloys can form a more protective and denser passive film on the metallic glass surface than the crystalline materials. In addition, the mechanical performance of the Ti-Zr-Si TFMGs is better than the crystalline counterparts. As a result, the Ti-based TFMGs are considered to be potential materials for bio-coating applications.

  1. Scanning droplet cell for high throughput electrochemical and photoelectrochemical measurements.

    PubMed

    Gregoire, John M; Xiang, Chengxiang; Liu, Xiaonao; Marcin, Martin; Jin, Jian

    2013-02-01

    High throughput electrochemical techniques are widely applied in material discovery and optimization. For many applications, the most desirable electrochemical characterization requires a three-electrode cell under potentiostat control. In high throughput screening, a material library is explored by either employing an array of such cells, or rastering a single cell over the library. To attain this latter capability with unprecedented throughput, we have developed a highly integrated, compact scanning droplet cell that is optimized for rapid electrochemical and photoeletrochemical measurements. Using this cell, we screened a quaternary oxide library as (photo)electrocatalysts for the oxygen evolution (water splitting) reaction. High quality electrochemical measurements were carried out and key electrocatalytic properties were identified for each of 5456 samples with a throughput of 4 s per sample. PMID:23464227

  2. In Situ Characterization of Triboelectrochemical Effects on Topography of Patterned Copper Surfaces

    NASA Astrophysics Data System (ADS)

    Joo, Sukbae; Liang, Hong

    2013-06-01

    The topographic response of patterned copper surfaces to chemical-mechanical polishing (CMP) was investigated using a triboelectrochemical approach. Experimental methods include using a combined system containing a tribometer and a potentiostat. Results showed that more step height reduction and lower average surface roughness were obtained via CMP in acidic than in alkaline slurry. The increased contact area between wafer, pad, and abrasives was associated with the increase in friction. It was found that pH-dependent oxide formation and removal dominate the step height reduction for both acidic and alkaline slurries. The in situ approach pinpointed interactions between mechanical stimulation, chemical reaction, and electrochemical passivation. This research is beneficial to understanding triboelectrochemistry in Cu chemical-mechanical polishing of patterned wafers, an important application in semiconductor manufacturing.

  3. A light emitting diode based photoelectrochemical screener for distributed combinatorial materials discovery

    NASA Astrophysics Data System (ADS)

    Winkler, Gates R.; Winkler, Jay R.

    2011-11-01

    Combinatorial approaches for targeted discovery of new materials require rapid screening systems to evaluate large numbers of new material compositions. High-throughput combinatorial materials discovery is a capital-intensive undertaking requiring sophisticated robotic sample preparation and rapid screening assays. A distributed approach to combinatorial materials discovery can achieve similar goals by increasing the breadth of participation and reducing the size of the capital investment. The discovery of new photoactive materials for solar fuels production demands a screening device to probe materials for electrochemical current production upon irradiation with visible light. We have developed a system that uses an array of pulsed light-emitting diodes (LEDs) synchronized with a two-electrode potentiostat that can measure the photoelectrochemical responses of combinatorial sample arrays deposited on conducting glass plates. Compared to raster scanning methods, this LED system trades spatial resolution for a substantial reduction in scan time.

  4. Optimization of hydrogen uptake in Ag-CNTs electrodes with charge-discharge cyclic currents

    NASA Astrophysics Data System (ADS)

    Khoshnevisan, B.; Behpour, M.; Kaveh, D.

    2009-06-01

    Electrochemical storage of hydrogen in Ag-CNTs (silver and carbon nanotubes) electrodes has been studied by potentiostat/galvanostat method. Foamed silver has been employed as a mattress for the CNTs and it caused better connections between CNTs and the silver. Therefore the enhancements in the hydrogen storage capacities have been justified. Acidic and thermal methods have been used for purifying the CNTs and the outputs have been characterized by XRD and Raman spectroscopy. It has been observed that in cyclic charge and discharge (C&D) procedures the amount of stored hydrogen in the electrodes (the discharge capacity) is very sensitive to the cyclic regulated currents and it is shown that the optimum value is about 326 mA h/g at 9 mA. This optimization can be attributed to two competitive phenomena: (i) re-alignment of the CNTs, and (ii) oxidation of the electrode's surface.

  5. Microstructure and properties of ultrafine grain nickel 200 after hydrostatic extrusion processes

    NASA Astrophysics Data System (ADS)

    Sitek, R.; Krajewski, C.; Kamiński, J.; Spychalski, M.; Garbacz, H.; Pachla, W.; Kurzydłowski, K. J.

    2012-09-01

    This paper presents the results of the studies of the structure and properties of ultrafine grained nickel 200 obtained by hydrostatic extrusion processes. Microstructure was characterized by means of optical microscopy and electron transmission microscopy. Corrosion resistance was studied by impedance and potentiodynamic methods using an AutoLab PGSTAT 100 potentiostat in 0.1 M Na2SO4 solution and in acidified (by addition of H2SO4) 0.1 M NaCl solution at pH = 4.2 at room temperature. Microhardness tests were also performed. The results showed that hydrostatic extrusion produces a heterogeneous, ultrafine-grained microstructure in nickel 200. The corrosive resistance tests showed that the grain refinement by hydrostatic extrusion is accompanied by a decreased corrosive resistance of nickel 200.

  6. Biocompatibility of nanotube formed Ti-30Nb-7Ta alloys.

    PubMed

    Kim, Eun-Sil; Choe, Han-Cheol

    2014-11-01

    The purpose of this study was to investigate the biocompatibility of Ti-30Nb-7Ta alloy surface decorated with TiO2 nanotubes by anodization in an electrolyte containing 1 M H3PO4 and 0.8 wt.% NaF with an applied voltage of 10 V for 2 h. The anodization was carried out using a scanning potentiostat. The microstructures of alloys and morphology of the nanotubes were investigated by optical microscopy, field emission scanning electron microscopy, and X-ray diffractometry. In comparison to the Ti-30Nb-3Ta alloy, the Ti-30Nb-7Ta alloy contained a lower amount of α" phase, while the β phase was higher. In this study, we observed the formation of a spongy porous layer on the Ti-30Nb-7Ta alloy, while the Ti-30Nb and Ti-30Nb-3Ta alloys showed an absence of such a spongy layer. PMID:25958540

  7. Polypyrrole/gold bilayer characterization

    NASA Astrophysics Data System (ADS)

    Fanning, Steven; Liu, Yingkai; Christophersen, Marc; Duerkop, Matthias; Smela, Elisabeth; Shapiro, Benjamin

    2005-05-01

    Polypyrrole/gold bilayer microactuators are being developed in our laboratory for biomedical applications such as microvalves. To fully open and close the valves, the bilayer hinges must be able to rotate between 0° and 180° within a few seconds against external forces. The layer thicknesses and hinge lengths must therefore be properly designed for the application. However, existing models fail to predict the correct behavior of microfabricated PPy/Au bilayer microactuators. Therefore, additional experimental data are needed to correctly forecast their performance. Bilayer actuators were fabricated with ranges of PPy thicknesses and hinge lengths. Bending angles were recorded through a stereomicroscope in the fully oxidized and reduced states. Isometric forces exerted by the hinges were measured with a force transducer, the output of which was read by a potentiostat and correlated with the applied potentials.

  8. A microfluidic paper-based electrochemical biosensor array for multiplexed detection of metabolic biomarkers

    NASA Astrophysics Data System (ADS)

    Zhao, Chen; Thuo, Martin M.; Liu, Xinyu

    2013-10-01

    Paper-based microfluidic devices have emerged as simple yet powerful platforms for performing low-cost analytical tests. This paper reports a microfluidic paper-based electrochemical biosensor array for multiplexed detection of physiologically relevant metabolic biomarkers. Different from existing paper-based electrochemical devices, our device includes an array of eight electrochemical sensors and utilizes a handheld custom-made electrochemical reader (potentiostat) for signal readout. The biosensor array can detect several analytes in a sample solution and produce multiple measurements for each analyte from a single run. Using the device, we demonstrate simultaneous detection of glucose, lactate and uric acid in urine, with analytical performance comparable to that of the existing commercial and paper-based platforms. The paper-based biosensor array and its electrochemical reader will enable the acquisition of high-density, statistically meaningful diagnostic information at the point of care in a rapid and cost-efficient way.

  9. Electrochemical fabrication and characterization of nanocontacts and nm-sized gaps

    NASA Astrophysics Data System (ADS)

    Mészáros, G.; Kronholz, S.; Karthäuser, S.; Mayer, D.; Wandlowski, T.

    2007-06-01

    Copper nanocontacts and molecular-sized nanogaps were prepared and characterized at electrified solid/liquid interfaces employing lithographic and electrochemical techniques. A dedicated four-electrode potentiostat was developed for controlling the electrochemical fabrication process and for monitoring the electrical characteristics of the nanostructures created. The formation and breaking of Cu nanocontacts exhibits conductance quantization characteristics. The statistical analysis of conductance histograms revealed a preferential stability of nanocontacts with integer values of G0, with a clear preference for 1 G0, 2 G0 and 3 G0. The growth of molecular-sized gaps shows quantized tunneling current, which is attributed to the discrete nature of Cu atoms, water molecules, and specifically adsorbed ions.

  10. Microdialysis sampling coupled to microchip electrophoresis with integrated amperometric detection on an all-glass substrate.

    PubMed

    Scott, David E; Grigsby, Ryan J; Lunte, Susan M

    2013-07-22

    The development of an all-glass separation-based sensor using microdialysis coupled to microchip electrophoresis with amperometric detection is described. The system includes a flow-gated interface to inject discrete sample plugs from the microdialysis perfusate into the microchip electrophoresis system. Electrochemical detection was accomplished with a platinum electrode in an in-channel configuration using a wireless electrically isolated potentiostat. To facilitate bonding around the in-channel electrode, a fabrication process was employed that produced a working and a reference electrode flush with the glass surface. Both normal and reversed polarity separations were performed with this sensor. The system was evaluated in vitro for the continuous monitoring of the production of hydrogen peroxide from the reaction of glucose oxidase with glucose. Microdialysis experiments were performed using a BASi loop probe with an overall lag time of approximately five minutes and a rise time of less than 60 seconds. PMID:23794474

  11. An economical and convenient experiment setup for electrode investigation.

    PubMed

    Aryan, Naser Pour; Rieger, Viola; Brendler, Christian; Rothermel, Albrecht

    2012-01-01

    Electrodes are among the critical components of neural stimulation devices. Investigating electrode properties like electrode impedance, charge injection capacity, and electrode corrosion limits plays an important role in electrode development. There are many commercial devices available for this purpose. Although useful, these devices are usually expensive and often offer more functions than required. We propose a versatile setup, composed of a LabVIEW program, a National Instruments multifunctional board, and a circuit built of discrete commercial elements. The system offers basic functions used in electrochemical investigation like current and voltage injection, cyclic voltammetry, and impedance spectroscopy. It offers the functionalities of both a potentiostat and an arbitrary waveform generator. It has already been applied elsewhere. PMID:23366017

  12. Electrochemical self-assembly of oriented zinc oxide film from polyethylene oxide containing electrolyte.

    PubMed

    Ju, Xiaohui; Feng, Wei; Fujii, Akihiko; Ozaki, Masanori

    2009-03-01

    Oriented nanopillar ZnO crystals were firstly fabricated by the potentiostatic cathodic electrodeposition technique on conducting glass substrates from polyethylene oxide (PEO) containing zinc nitrate solutions at low temperature (343 K). The mechanism for PEO-assisted electrochemical growth of ZnO hexagonal columus was proposed and confirmed by scanning electron microscopy, X-ray diffraction and UV-visible spectrophotometer measurements. It was observed that the concentration of PEO played an important role in the morphology and size of ZnO crystals. The structure and optical studies indicated that the addition of PEO not only influenced crystal growth habit but also improve the optical properties of ZnO. PMID:19435038

  13. Reduction mechanism of sulfur in lithium-sulfur battery: From elemental sulfur to polysulfide

    DOE PAGESBeta

    Zheng, Dong; Yang, Xuran; Zhang, Xiaoqing; Wang, Jiankun; Qu, Deyu; Qu, Deyang

    2015-10-30

    In this study, the polysulfide ions formed during the first reduction wave of sulfur in Li–S battery were determined through both in-situ and ex-situ derivatization of polysulfides. By comparing the cyclic voltammetric results with and without the derivatization reagent (methyl triflate) as well as the in-situ and ex-situ derivatization results under potentiostatic condition, in-situ derivatization was found to be more appropriate than its ex-situ counterpart, since subsequent fast chemical reactions between the polysulfides and sulfur may occur during the timeframe of ex-situ procedures. It was found that the major polysulfide ions formed at the first reduction wave of elemental sulfurmore » were the S42– and S52– species, while the widely accepted reduction products of S82– and S62– for the first reduction wave were in low abundance.« less

  14. Considerations on electrical impedance measurements of electrolyte solutions in a four-electrode cell

    NASA Astrophysics Data System (ADS)

    Chaparro, C. V.; Herrera, L. V.; Meléndez, A. M.; Miranda, D. A.

    2016-02-01

    A tetrapolar probe to measure the electrical properties of electrolyte solutions was implemented with gold electrodes according to the van der Pauw method. Electrical impedance spectroscopy (EIS) measurements of different concentrations of phosphate buffer saline (PBS) solution and an oral mucosal tissue sample dispersed in PBS were performed in the galvanostatic mode using a four-electrode cell (tetrapolar probe). Taking advantage of using a potentiostat/galvanostat for carrying out the electrical measurements, a simple and rapid method using a three-electrode electrochemical cell is described for: a) cleaning of electrodes, b) verification of surface chemical state of electrode material and c) choice of current supplied to electrodes for EIS measurements. Results of this research shown a depolarization effect due to the addition of oral mucosa tissue cells into the PBS solution.

  15. Photoelectrochemical and Electrochemical Characterization of Sub-Micro-Gram Amounts of Organic Semiconductors Using Scanning Droplet Cell Microscopy.

    PubMed

    Kollender, Jan Philipp; Gasiorowski, Jacek; Sariciftci, Niyazi S; Mardare, Andrei I; Hassel, Achim Walter

    2014-07-31

    A model organic semiconductor (MDMO-PPV) was used for testing a modified version of a photoelectrochemical scanning droplet cell microscope (PE-SDCM) adapted for use with nonaqueous electrolytes and containing an optical fiber for localized illumination. The most attractive features of the PE-SDCM are represented by the possibility of addressing small areas on the investigated substrate and the need of small amounts of electrolyte. A very small amount (ng) of the material under study is sufficient for a complete electrochemical and photoelectrochemical characterization due to the scanning capability of the cell. The electrochemical behavior of the polymer was studied in detail using potentiostatic and potentiodynamic investigations as well as electrochemical impedance spectroscopy. Additionally, the photoelectrochemical properties were investigated under illumination conditions, and the photocurrents found were at least 3 orders of magnitude higher than the dark (background) current, revealing the usefulness of this compact microcell for photovoltaic characterizations. PMID:25101149

  16. Redox mechanism in the binary transition metal phosphide Cu3P

    NASA Astrophysics Data System (ADS)

    Mauvernay, B.; Doublet, M.-L.; Monconduit, L.

    2006-05-01

    The electrochemical behaviour of the binary transition metal phosphide Cu3P towards lithium is investigated through galvano- and potentiostatic measurements. Obtained through high-temperature synthesis, this system shows a better volumetric capacity than graphite and a good capacity retention. In situ X-ray diffraction and first-principles electronic structure calculations are combined with the electrochemical results to show that the complete insertion of 3Li+ in the Cu3P electrode proceeds with the formation of three intermediate phases of lithium composition LixCu(3-x)P (x=1,2,3). The extra capacity previously observed in discharge is now clearly assigned to lithium insertion into the CuP2 impurity and to SEI reactions.

  17. Tribo-electrochemical characterization of hafnium multilayer systems deposited on nitride/vanadium nitride AISI 4140 steel

    NASA Astrophysics Data System (ADS)

    Mora, M.; Vera, E.; Aperador, W.

    2016-02-01

    In this work is presented the synergistic behaviour among corrosion/wear (tribocorrosion) of the multilayer coatings hafnium nitride/vanadium nitride [HfN/VN]n. The multilayers were deposited on AISI 4140 steel using the technique of physical vapor deposition PVD magnetron sputtering, the tests were performed using a pin-on-disk tribometer, which has an adapted potentiostat galvanostat with three-electrode electrochemical cell. Tribocorrosive parameters such as: Friction coefficient between the coating and the counter body (100 Cr6 steel ball); Polarization resistance by means of electrochemical impedance spectroscopy technique and corrosion rate by polarization curves were determined. It was observed an increase in the polarization resistance, a decrease in the corrosion rate and a low coefficient of friction in comparison with the substrate, due to an increase on the number of bilayers.

  18. Microdialysis Sampling Coupled to Microchip Electrophoresis with Integrated Amperometric Detection on an All Glass Substrate

    PubMed Central

    Scott, David E.; Grigsby, Ryan; Lunte, Susan M.

    2013-01-01

    The development of an all-glass separation-based sensor using microdialysis coupled to microchip electrophoresis with amperometric detection is described. The system includes a flow-gated interface to inject discrete sample plugs from the microdialysis perfusate into the microchip electrophoresis system. Electrochemical detection was accomplished with a platinum electrode in an in-channel configuration using a wireless electrically isolated potentiostat. To facilitate bonding around the in-channel electrode, a fabrication process was employed that produced a working and a reference electrode flush with the glass surface. Both normal and reversed polarity separations were performed with this sensor. The system was evaluated in vitro for the continuous monitoring of the production of hydrogen peroxide from the reaction of glucose oxidase with glucose. Microdialysis experiments were performed using a BASi loop probe with an overall lag time of approximately five minutes and a rise time of less than 60 seconds. PMID:23794474

  19. Self-organized highly ordered TiO{sub 2} nanotubes in organic aqueous system

    SciTech Connect

    Wan Jun; Yan Xia; Ding Junjie; Wang Meng; Hu Kongcheng

    2009-12-15

    A simple method to achieve self-organized, freestanding TiO{sub 2} nanotube array was constructed, free of corrosive etching process which was traditionally employed to separate TiO{sub 2} nanotubes from the metallic Ti substrate. The TiO{sub 2} nanotube arrays were constructed through potentiostatic anodization of Ti foil in aqueous electrolyte containing NH{sub 4}F and ethylene glycol. The nanotubes in the array were of 45 {mu}m lengths and 100 nm average pore diameters. The effect of NH{sub 4}F concentration on the length of the self-organized nanotube arrays was investigated. Electrochemical and spectroscopic measurements showed that the as-prepared nanotubes possessed large surface areas, good uniformity, and were ready for enzyme immobilization. The as-prepared nanotube arrays were amorphous, but crystallized with annealing at elevated temperatures, as demonstrated by X-ray diffraction (XRD).

  20. Corrosion resistance of polyurethane-coated nitinol cardiovascular stents.

    PubMed

    Mazumder, M M; De, S; Trigwell, S; Ali, N; Mazumder, M K; Mehta, J L

    2003-01-01

    Corrosion of metal stents implanted inside an artery can have two adverse effects: (1) tissue reaction and possible toxic effects from the metal ions leaching out of the stent, and (2) loss of mechanical strength of the stent caused by corrosion. The corrosion resistance of Nitinol (Nickel-Titanium) stents and its modulation with different film thickness of polymer coating was studied against an artificial physiological solution using a Potentiostat/Galvanostat and an electrochemical corrosion cell. The corrosion rate decreased rapidly from 275 microm/year for an uncoated surface down to less than 13 microm/year for a 30 microm thick polyurethane coating. Stainless steel (316L) and Nitinol both contain potentially toxic elements, and both are subject to stress corrosion. Minimization of corrosion can significantly reduce both tissue reaction and structural degradation. PMID:14870939

  1. Effect of annealing temperature on the pitting corrosion resistance of super duplex stainless steel UNS S32750

    SciTech Connect

    Tan Hua; Jiang Yiming; Deng Bo; Sun Tao; Xu Juliang; Li Jin

    2009-09-15

    The pitting corrosion resistance of commercial super duplex stainless steels SAF2507 (UNS S32750) annealed at seven different temperatures ranging from 1030 deg. C to 1200 deg. C for 2 h has been investigated by means of potentiostatic critical pitting temperature. The microstructural evolution and pit morphologies of the specimens were studied through optical/scanning electron microscope. Increasing annealing temperature from 1030 deg. C to 1080 deg. C elevates the critical pitting temperature, whereas continuing to increase the annealing temperature to 1200 deg. C decreases the critical pitting temperature. The specimens annealed at 1080 deg. C for 2 h exhibit the best pitting corrosion resistance with the highest critical pitting temperature. The pit morphologies show that the pit initiation sites transfer from austenite phase to ferrite phase as the annealing temperature increases. The aforementioned results can be explained by the variation of pitting resistance equivalent number of ferrite and austenite phase as the annealing temperature changes.

  2. A Fully Automated Sequential-Injection Analyser for Dual Electrogenerated Chemiluminescence/Amperometric Detection

    PubMed Central

    Nika, Maria

    2006-01-01

    This work describes the development of a dedicated, fully automated sequential-injection analysis (SIA) apparatus suitable for simultaneous electrogenerated chemiluminescence (ECL) and amperometric detection. The instrument is composed of a peristaltic pump, a multiposition selection valve, a home-made potentiostat, a thin-layer electrochemical/optical flow-through cell, and a light detector. Control of the experimental sequence and simultaneous data acquisition of the light and the current intensities were performed in LabVIEW6.1. The CL reagents and the sample were first aspirated as distinct zones into the holding coil of the analyser and, then, delivered to the cell; during their travel, the individual zones mixed and the ECL reaction was initiated as soon as the mixed regents reached the cell. The utility of the analyser was demonstrated for the detection of oxalate and H 2 O 2 based on their ECL reactions with Ru ( bpy ) 3 2 and luminol, respectively. PMID:17671622

  3. A fully automated sequential-injection analyser for dual electrogenerated chemiluminescence/amperometric detection.

    PubMed

    Economou, Anastasios; Nika, Maria

    2006-01-01

    This work describes the development of a dedicated, fully automated sequential-injection analysis (SIA) apparatus suitable for simultaneous electrogenerated chemiluminescence (ECL) and amperometric detection. The instrument is composed of a peristaltic pump, a multiposition selection valve, a home-made potentiostat, a thin-layer electrochemical/optical flow-through cell, and a light detector. Control of the experimental sequence and simultaneous data acquisition of the light and the current intensities were performed in LabVIEW6.1. The CL reagents and the sample were first aspirated as distinct zones into the holding coil of the analyser and, then, delivered to the cell; during their travel, the individual zones mixed and the ECL reaction was initiated as soon as the mixed regents reached the cell. The utility of the analyser was demonstrated for the detection of oxalate and H2O2 based on their ECL reactions with Ru(bpy)32 and luminol, respectively. PMID:17671622

  4. Synthesis of nano-structured polypyrrole/copper electrodes for nitrate and nitrite electroreduction

    NASA Astrophysics Data System (ADS)

    Phuong Thoa Nguyen, Thi; Thinh Nguyen, Viet; Nguyen Bui, Nhat; Do, Duong Kim Bao; Pham, Anh Minh

    2010-09-01

    Nanostructured polypyrrole film was synthesized onto a copper electrode in solutions of oxalic and salicylic acids and their buffers. The electrooxidation of pyrrole to form polypyrrole film and the electroreduction of nitrate and nitrite ions at synthesized Ppy modified copper electrodes (Ppy/Cu) in potassium chloride aqueous solutions were studied using chronoamperometry. The nanoporous structure of the synthesized Ppy films was characterized by scanning electron microscopy (SEM). Nitrate and nitrite reduction were performed by an electrochemical method under potentiostatic conditions. The Ppy/Cu electrodes prepared in the oxalate buffer and salicylic acid solutions perform more stable catalytic activity for nitrate reduction; their service life is about ten times longer than that for the electrodes prepared in oxalic acid solution. After 20?h of electrolysis, the nitrite was reduced completely with 100% efficiency and the nitrate was reduced with 35% efficiency. Report submitted to the 5th International Workshop on Advanced Materials Science and Nanotechnology IWAMSN, Hanoi, 9-12 November 2010.

  5. Electrocatalytic activities of cathode electrodes for water electrolysis using tetra-alkyl-ammonium-sulfonic acid ionic liquid as electrolyte

    NASA Astrophysics Data System (ADS)

    Fiegenbaum, Fernanda; de Souza, Michèle O.; Becker, Márcia R.; Martini, Emilse M. A.; de Souza, Roberto F.

    2015-04-01

    The hydrogen evolution reaction (HER) performed with platinum (Pt), nickel (Ni), stainless steel 304 (SS) or glassy carbon (GC) cathodes in 0.1 M 3-triethylammonium-propanesulfonic acid tetrafluoroborate (TEA-PS.BF4) solution is studied using quasi-potentiostatic and impedance spectroscopy techniques. The objective is to compare the catalytic effect on the cathode using different materials to obtain hydrogen by water electrolysis. Furthermore, the catalytic effect of the ionic liquid (IL) on the cathode compared with that of a hydrochloric acid (HCl) solution with same pH value (0.8) is reported. A low activation energy (Ea) of 8.7 kJ mol-1 is found for the glassy carbon cathode. Tafel plots obtained with TEA-PS.BF4 IL suggest the formation of an electroactive layer of IL on the cathode, which may be responsible for the catalytically enhanced performance observed.

  6. Simultaneous telemetric monitoring of brain glucose and lactate and motion in freely moving rats.

    PubMed

    Rocchitta, Gaia; Secchi, Ottavio; Alvau, Maria Domenica; Farina, Donatella; Bazzu, Gianfranco; Calia, Giammario; Migheli, Rossana; Desole, Maria Speranza; O'Neill, Robert D; Serra, Pier A

    2013-11-01

    A new telemetry system for simultaneous detection of extracellular brain glucose and lactate and motion is presented. The device consists of dual-channel, single-supply miniature potentiostat-I/V converter, a microcontroller unit, a signal transmitter, and a miniaturized microvibration sensor. Although based on simple and inexpensive components, the biotelemetry device has been used for accurate transduction of the anodic oxidation currents generated on the surface of implanted glucose and lactate biosensors and animal microvibrations. The device was characterized and validated in vitro before in vivo experiments. The biosensors were implanted in the striatum of freely moving animals and the biotelemetric device was fixed to the animal's head. Physiological and pharmacological stimulations were given in order to induce striatal neural activation and to modify the motor behavior in awake, untethered animals. PMID:24102201

  7. Effects of TiN coating on the corrosion of nanostructured Ti-30Ta-xZr alloys for dental implants

    NASA Astrophysics Data System (ADS)

    Kim, Won-Gi; Choe, Han-Cheol

    2012-01-01

    Electrochemical characteristics of a titanium nitride (TiN)-coated/nanotube-formed Ti-Ta-Zr alloy for biomaterials have been researched by using the magnetic sputter and electrochemical methods. Ti-30Ta-xZr (x = 3, 7 and 15 wt%) alloys were prepared by arc melting and heat treated for 24 h at 1000 °C in an argon atmosphere and then water quenching. The formation of oxide nanotubes was achieved by anodizing a Ti-30Ta-xZr alloy in H3PO4 electrolytes containing small amounts of fluoride ions at room temperature. Anodization was carried out using a scanning potentiostat, and all experiments were conducted at room temperature. The microstructure and morphology of nanotube arrays were characterized by optical microscopy (OM), field emission scanning electron microscopy (FE-SEM) and X-ray diffraction (XRD). The TiN coatings were obtained by the radio-frequency (RF) magnetron sputtering technique. The depositions were performed from pure Ti targets on Ti-30Ta-xZr alloys substrates. The corrosion properties of the specimens were examined using potentiodynamic test in a 0.9% NaCl solution by using potentiostat. The microstructures of Ti-30Ta-xZr alloys were changed from an equiaxed to a needle-like structure with increasing Zr content. The interspace between the nanotubes was approximately 20, 80 and 200 nm for Zr contents of 3, 7 and 15 wt%, respectively. The corrosion resistance of the TiN-coated on the anodized Ti-30Ta-xZr alloys was higher than that of the untreated Ti alloys, indicating a better protective effect.

  8. Analysis of electrochemical noise from metastable pitting in aluminum, aged Al-2%Cu, and AA 2024-T3

    SciTech Connect

    Pride, S.T.; Scully, J.R.; Hudson, J.L.

    1996-12-31

    The authors compare methods of analyzing electrochemical current (ECN) and potential (EPN) noise data associated with metastable pitting and the transition from metastable to stable pitting. Various analysis methods were applied to electrochemical noise data associated with metastable pit events on aluminum, aged Al-2%Cu, and AA 2024-T3 ST. Two experimental approaches were used. High-purity Al, roughly simulating copper-depleted grain boundary zones in aged Al-Cu alloys, was potentiostatically polarized so that current spikes associated with individual pitting events could be analyzed. Second, the coupling current between nominally identical galvanically coupled Al, aged Al-2%Cu, and AA 2024-T3 ST electrodes was recorded in conjunction with couple potential using a saturated calomel reference electrode. Pit stabilization occurred when individual pits exceeded a threshold of I{sub pit}/r{sub pit} > 10{sup {minus}2} A/cm at all times during pit growth as established from potentiostatic measurements. The magnitude of this ratio is linked directly to the concentration of the aggressive solution within pits. Two related statistical pit stabilization factors (I{sub rms}/r{sub pit total} from ECN data and the mean of (I{sub peak}-I{sub ox})/r{sub pit} values from each pit current spike) were obtained from galvanic ECN data containing a large number of pit current spikes. These parameters provided a better indication of the transition to stable pitting than the pitting index or noise resistance but also had shortcomings. Spectral analysis using current and potential spectral power density (SPD) data provided qualitative information on pit susceptibility. However, the transition to stable pitting could not be accurately defined because of a lack of information on pit sizes in spectral data.

  9. Nanopore formation on the surface oxide of commercially pure titanium grade 4 using a pulsed anodization method in sulfuric acid.

    PubMed

    Williamson, R S; Disegi, J; Griggs, J A; Roach, M D

    2013-10-01

    Titanium and its alloys form a thin amorphous protective surface oxide when exposed to an oxygen environment. The properties of this oxide layer are thought to be responsible for titanium and its alloys biocompatibility, chemical inertness, and corrosion resistance. Surface oxide crystallinity and pore size are regarded to be two of the more important properties in establishing successful osseointegration. Anodization is an electrochemical method of surface modification used for colorization marking and improved bioactivity on orthopedic and dental titanium implants. Research on titanium anodization using sulphuric acid has been reported in the literature as being primarily conducted in molarity levels 3 M and less using either galvanostatic or potentiostatic methods. A wide range of pore diameters ranging from a few nanometers up to 10 μm have been shown to form in sulfuric acid electrolytes using the potentiostatic and galvanostatic methods. Nano sized pores have been shown to be beneficial for bone cell attachment and proliferation. The purpose of the present research was to investigate oxide crystallinity and pore formation during titanium anodization using a pulsed DC waveform in a series of sulfuric acid electrolytes ranging from 0.5 to 12 M. Anodizing titanium in increasing sulfuric acid molarities showed a trend of increasing transformations of the amorphous natural forming oxide to the crystalline phases of anatase and rutile. The pulsed DC waveform was shown to produce pores with a size range from ≤0.01 to 1 μm(2). The pore size distributions produced may be beneficial for bone cell attachment and proliferation. PMID:23807314

  10. Statistic analysis of operational influences on the cold start behaviour of PEM fuel cells

    NASA Astrophysics Data System (ADS)

    Oszcipok, M.; Riemann, D.; Kronenwett, U.; Kreideweis, M.; Zedda, M.

    For portable fuel cell systems a multitude of applications have been presented over the past few years. Most of these applications were developed for indoor use, and not optimised for outdoor conditions. The key problem concerning this case is the cold start ability of the polymer electrolyte membrane fuel cell (PEMFC). This topic was first investigated by the automotive industry, which has the same requirements for alternative traction systems as for conventional combustion engines. The technical challenge is the fact that produced water freezes to ice after shut-down of the PEMFC and during start-up when the temperature is below 0 °C. To investigate the basic cold start behaviour isothermal, potentiostatic single cell experiments were performed and the results are presented. The cold start behaviour is evaluated using the calculated cumulated charge transfer through the membrane which directly corresponds with the amount of produced water in the PEMFC. The charge transfer curves were mathematically fitted to obtain only three parameters describing the cold start-up with the cumulated charge transfer density and the results are analysed using the statistical software Cornerstone 4.0. The results of the statistic regression analyses are used to establish a statistic-based prediction model of the cold start behaviour which describes the behaviour of the current density during the experiment. The regression shows that the initial start current mainly depends on the membrane humidity and the operation voltage. After the membrane humidity has reached its maximum, the current density drops down to zero. The current decay also depends on the constant gas flows of the reactant gases. Ionic conductivity of the membrane and charge transfer resistance were investigated by a series of ac impedance spectra during potentiostatic operation of the single cell at freezing temperatures. Cyclic voltammetry and polarisation curves between cold start experiments show degradation effects by ice formation in the porous structures which lead to significant performance loss.

  11. Electrochemically and bioelectrochemically induced ammonium recovery.

    PubMed

    Gildemyn, Sylvia; Luther, Amanda K; Andersen, Stephen J; Desloover, Joachim; Rabaey, Korneel

    2015-01-01

    Streams such as urine and manure can contain high levels of ammonium, which could be recovered for reuse in agriculture or chemistry. The extraction of ammonium from an ammonium-rich stream is demonstrated using an electrochemical and a bioelectrochemical system. Both systems are controlled by a potentiostat to either fix the current (for the electrochemical cell) or fix the potential of the working electrode (for the bioelectrochemical cell). In the bioelectrochemical cell, electroactive bacteria catalyze the anodic reaction, whereas in the electrochemical cell the potentiostat applies a higher voltage to produce a current. The current and consequent restoration of the charge balance across the cell allow the transport of cations, such as ammonium, across a cation exchange membrane from the anolyte to the catholyte. The high pH of the catholyte leads to formation of ammonia, which can be stripped from the medium and captured in an acid solution, thus enabling the recovery of a valuable nutrient. The flux of ammonium across the membrane is characterized at different anolyte ammonium concentrations and currents for both the abiotic and biotic reactor systems. Both systems are compared based on current and removal efficiencies for ammonium, as well as the energy input required to drive ammonium transfer across the cation exchange membrane. Finally, a comparative analysis considering key aspects such as reliability, electrode cost, and rate is made. This video article and protocol provide the necessary information to conduct electrochemical and bioelectrochemical ammonia recovery experiments. The reactor setup for the two cases is explained, as well as the reactor operation. We elaborate on data analysis for both reactor types and on the advantages and disadvantages of bioelectrochemical and electrochemical systems. PMID:25651406

  12. The electrochemical behavior and surface analysis of Ti49.6Ni45.1Cu5Cr0.3 alloy for orthodontic usage.

    PubMed

    Zheng, Y-F; Wang, Q Y; Li, L

    2008-08-01

    The aim of this study was to investigate the electrochemical behavior of Ti(49.6)Ni(45.1)Cu(5)Cr(0.3) (TiNiCuCr) alloy in artificial saliva solutions with a wide rage of pH values and to characterize the surface passive film after polarization tests. This article represents the ideal, static environment and associated electrochemical response and comparison values. The corrosion behavior of TiNiCuCr alloy was systematically studied by open circuit potential, potentiodynamic, potentiostatic, and electrochemical impedance techniques. Potentiodynamic and potentiostatic test results showed that the corrosion behavior of TiNiCuCr was similar to that of NiTi alloy. Both corrosion potential (E(corr)) and pitting corrosion potential (E(b)) showed a pH-dependent tendency that E(corr) and E(b) decreased with the increase of the pH value. X-ray photoelectron spectroscopy results revealed the composition of the passive film consisted mainly of TiO(2) with a little amount of Ni oxides (NiO/Ni(2)O(3)) that was identical with NiTi alloy. Besides Ni, a Cu enriched sub-layer was also found. The nickel ion release rate showed a typical time-related decrease as examined by ICP/OES. In conclusion, the addition of Cu and Cr had little effect on the corrosion behavior of NiTi or on the composition and the structure of the passive film. PMID:18161810

  13. Real-time telemetry system for amperometric and potentiometric electrochemical sensors.

    PubMed

    Wang, Wei-Song; Huang, Hong-Yi; Chen, Shu-Chun; Ho, Kuo-Chuan; Lin, Chia-Yu; Chou, Tse-Chuan; Hu, Chih-Hsien; Wang, Wen-Fong; Wu, Cheng-Feng; Luo, Ching-Hsing

    2011-01-01

    A real-time telemetry system, which consists of readout circuits, an analog-to-digital converter (ADC), a microcontroller unit (MCU), a graphical user interface (GUI), and a radio frequency (RF) transceiver, is proposed for amperometric and potentiometric electrochemical sensors. By integrating the proposed system with the electrochemical sensors, analyte detection can be conveniently performed. The data is displayed in real-time on a GUI and optionally uploaded to a database via the Internet, allowing it to be accessed remotely. An MCU was implemented using a field programmable gate array (FPGA) to filter noise, transmit data, and provide control over peripheral devices to reduce power consumption, which in sleep mode is 70 mW lower than in operating mode. The readout circuits, which were implemented in the TSMC 0.18-?m CMOS process, include a potentiostat and an instrumentation amplifier (IA). The measurement results show that the proposed potentiostat has a detectable current range of 1 nA to 100 ?A, and linearity with an R2 value of 0.99998 in each measured current range. The proposed IA has a common-mode rejection ratio (CMRR) greater than 90 dB. The proposed system was integrated with a potentiometric pH sensor and an amperometric nitrite sensor for in vitro experiments. The proposed system has high linearity (an R2 value greater than 0.99 was obtained in each experiment), a small size of 5.6 cm 8.7 cm, high portability, and high integration. PMID:22164093

  14. A combined electrochemical and optical trapping platform for measuring single cell respiration rates at electrode interfaces

    NASA Astrophysics Data System (ADS)

    Gross, Benjamin J.; El-Naggar, Mohamed Y.

    2015-06-01

    Metal-reducing bacteria gain energy by extracellular electron transfer to external solids, such as naturally abundant minerals, which substitute for oxygen or the other common soluble electron acceptors of respiration. This process is one of the earliest forms of respiration on earth and has significant environmental and technological implications. By performing electron transfer to electrodes instead of minerals, these microbes can be used as biocatalysts for conversion of diverse chemical fuels to electricity. Understanding such a complex biotic-abiotic interaction necessitates the development of tools capable of probing extracellular electron transfer down to the level of single cells. Here, we describe an experimental platform for single cell respiration measurements. The design integrates an infrared optical trap, perfusion chamber, and lithographically fabricated electrochemical chips containing potentiostatically controlled transparent indium tin oxide microelectrodes. Individual bacteria are manipulated using the optical trap and placed on the microelectrodes, which are biased at a suitable oxidizing potential in the absence of any chemical electron acceptor. The potentiostat is used to detect the respiration current correlated with cell-electrode contact. We demonstrate the system with single cell measurements of the dissimilatory-metal reducing bacterium Shewanella oneidensis MR-1, which resulted in respiration currents ranging from 15 fA to 100 fA per cell under our measurement conditions. Mutants lacking the outer-membrane cytochromes necessary for extracellular respiration did not result in any measurable current output upon contact. In addition to the application for extracellular electron transfer studies, the ability to electronically measure cell-specific respiration rates may provide answers for a variety of fundamental microbial physiology questions.

  15. Power management systems for sediment microbial fuel cells in high power and continuous power applications

    NASA Astrophysics Data System (ADS)

    Donovan, Conrad Koble

    The objective of this dissertation was to develop power management systems (PMS) for sediment microbial fuel cells (SFMCs) for high power and continuous applications. The first part of this dissertation covers a new method for testing the performance of SMFCs. This device called the microbial fuel cell tester was developed to automatically test power generation of PMS. The second part focuses on a PMS capable of delivering high power in burst mode. This means that for a small amount of time a large amount of power up to 2.5 Watts can be delivered from a SMFC only generating mW level power. The third part is aimed at developing a multi-potentiostat laboratory tool that measures the performance at fixed cell potentials of microbial fuel cells so that I can optimize them for use with the PMS. This tool is capable of controlling the anode potential or cathode potential and measuring current of six separate SMFCs simultaneously. By operating multiple potentiostats, I was able to run experiments that find ideal operating conditions for the sediment microbial fuel cells, and also I can optimize the power management system for these conditions. The fourth part of the dissertation is targeting a PMS that was able to operate a sensor continuously which was powered by an SMFC. In pervious applications involving SMFCs, the PMS operated in batch mode. In this PMS, the firmware on the submersible ultrasonic receiver (SUR) was modified for use with my PMS. This integration of PMS and SUR allowed for the continuous operation of the SUR without using a battery. Finally, the last part of the dissertation recommends a scale-up power management system to overcome the linearity scale up issue of SMFCs as future work. Concluding remarks are also added to summarize the goal and focus of this dissertation.

  16. A combined electrochemical and optical trapping platform for measuring single cell respiration rates at electrode interfaces.

    PubMed

    Gross, Benjamin J; El-Naggar, Mohamed Y

    2015-06-01

    Metal-reducing bacteria gain energy by extracellular electron transfer to external solids, such as naturally abundant minerals, which substitute for oxygen or the other common soluble electron acceptors of respiration. This process is one of the earliest forms of respiration on earth and has significant environmental and technological implications. By performing electron transfer to electrodes instead of minerals, these microbes can be used as biocatalysts for conversion of diverse chemical fuels to electricity. Understanding such a complex biotic-abiotic interaction necessitates the development of tools capable of probing extracellular electron transfer down to the level of single cells. Here, we describe an experimental platform for single cell respiration measurements. The design integrates an infrared optical trap, perfusion chamber, and lithographically fabricated electrochemical chips containing potentiostatically controlled transparent indium tin oxide microelectrodes. Individual bacteria are manipulated using the optical trap and placed on the microelectrodes, which are biased at a suitable oxidizing potential in the absence of any chemical electron acceptor. The potentiostat is used to detect the respiration current correlated with cell-electrode contact. We demonstrate the system with single cell measurements of the dissimilatory-metal reducing bacterium Shewanella oneidensis MR-1, which resulted in respiration currents ranging from 15 fA to 100 fA per cell under our measurement conditions. Mutants lacking the outer-membrane cytochromes necessary for extracellular respiration did not result in any measurable current output upon contact. In addition to the application for extracellular electron transfer studies, the ability to electronically measure cell-specific respiration rates may provide answers for a variety of fundamental microbial physiology questions. PMID:26133851

  17. High-efficiency synergistic conversion of CO2 to methanol using Fe2O3 nanotubes modified with double-layer Cu2O spheres

    NASA Astrophysics Data System (ADS)

    Li, Peiqiang; Jing, Hua; Xu, Jinfeng; Wu, Chenxiao; Peng, Hui; Lu, Jing; Lu, Fusui

    2014-09-01

    Cuprous oxide/hematite nanotubes (Cu2O/Fe2O3NTs) were prepared by a potentiostatic electrodeposited method, in which different structured Cu2O materials were modified onto Fe2O3 NTs surface. Among them, the material with double-layer Cu2O spheres (Cu2O/Fe2O3 NTs-30) showed excellent photoelectrocatalytic (PEC) properties with a suitable energy band gap (1.96 eV) and a smaller overpotential (0.18 V). Furthermore, Cu2O/Fe2O3 NTs-30 showed two types of synergisms in the PEC reduction of CO2: (i) between electrocatalysis and photocatalysis and (ii) between Cu2O and Fe2O3NTs. The faradaic efficiency and methanol yield reached 93% and 4.94 mmol L-1 cm-2 after 6 h, respectively.Cuprous oxide/hematite nanotubes (Cu2O/Fe2O3NTs) were prepared by a potentiostatic electrodeposited method, in which different structured Cu2O materials were modified onto Fe2O3 NTs surface. Among them, the material with double-layer Cu2O spheres (Cu2O/Fe2O3 NTs-30) showed excellent photoelectrocatalytic (PEC) properties with a suitable energy band gap (1.96 eV) and a smaller overpotential (0.18 V). Furthermore, Cu2O/Fe2O3 NTs-30 showed two types of synergisms in the PEC reduction of CO2: (i) between electrocatalysis and photocatalysis and (ii) between Cu2O and Fe2O3NTs. The faradaic efficiency and methanol yield reached 93% and 4.94 mmol L-1 cm-2 after 6 h, respectively. Electronic supplementary information (ESI) available: High-efficiency synergistic conversion of CO2 to methanol using Fe2O3 nanotubes modified with double-layer Cu2O spheres. See DOI: 10.1039/c4nr02902j

  18. A combined electrochemical and optical trapping platform for measuring single cell respiration rates at electrode interfaces

    SciTech Connect

    Gross, Benjamin J.; El-Naggar, Mohamed Y.

    2015-06-15

    Metal-reducing bacteria gain energy by extracellular electron transfer to external solids, such as naturally abundant minerals, which substitute for oxygen or the other common soluble electron acceptors of respiration. This process is one of the earliest forms of respiration on earth and has significant environmental and technological implications. By performing electron transfer to electrodes instead of minerals, these microbes can be used as biocatalysts for conversion of diverse chemical fuels to electricity. Understanding such a complex biotic-abiotic interaction necessitates the development of tools capable of probing extracellular electron transfer down to the level of single cells. Here, we describe an experimental platform for single cell respiration measurements. The design integrates an infrared optical trap, perfusion chamber, and lithographically fabricated electrochemical chips containing potentiostatically controlled transparent indium tin oxide microelectrodes. Individual bacteria are manipulated using the optical trap and placed on the microelectrodes, which are biased at a suitable oxidizing potential in the absence of any chemical electron acceptor. The potentiostat is used to detect the respiration current correlated with cell-electrode contact. We demonstrate the system with single cell measurements of the dissimilatory-metal reducing bacterium Shewanella oneidensis MR-1, which resulted in respiration currents ranging from 15 fA to 100 fA per cell under our measurement conditions. Mutants lacking the outer-membrane cytochromes necessary for extracellular respiration did not result in any measurable current output upon contact. In addition to the application for extracellular electron transfer studies, the ability to electronically measure cell-specific respiration rates may provide answers for a variety of fundamental microbial physiology questions.

  19. Real-Time Telemetry System for Amperometric and Potentiometric Electrochemical Sensors

    PubMed Central

    Wang, Wei-Song; Huang, Hong-Yi; Chen, Shu-Chun; Ho, Kuo-Chuan; Lin, Chia-Yu; Chou, Tse-Chuan; Hu, Chih-Hsien; Wang, Wen-Fong; Wu, Cheng-Feng; Luo, Ching-Hsing

    2011-01-01

    A real-time telemetry system, which consists of readout circuits, an analog-to-digital converter (ADC), a microcontroller unit (MCU), a graphical user interface (GUI), and a radio frequency (RF) transceiver, is proposed for amperometric and potentiometric electrochemical sensors. By integrating the proposed system with the electrochemical sensors, analyte detection can be conveniently performed. The data is displayed in real-time on a GUI and optionally uploaded to a database via the Internet, allowing it to be accessed remotely. An MCU was implemented using a field programmable gate array (FPGA) to filter noise, transmit data, and provide control over peripheral devices to reduce power consumption, which in sleep mode is 70 mW lower than in operating mode. The readout circuits, which were implemented in the TSMC 0.18-μm CMOS process, include a potentiostat and an instrumentation amplifier (IA). The measurement results show that the proposed potentiostat has a detectable current range of 1 nA to 100 μA, and linearity with an R2 value of 0.99998 in each measured current range. The proposed IA has a common-mode rejection ratio (CMRR) greater than 90 dB. The proposed system was integrated with a potentiometric pH sensor and an amperometric nitrite sensor for in vitro experiments. The proposed system has high linearity (an R2 value greater than 0.99 was obtained in each experiment), a small size of 5.6 cm × 8.7 cm, high portability, and high integration. PMID:22164093

  20. Silver(I) ions ultrasensitive detection at carbon electrodes-analysis of waters, tobacco cells and fish tissues.

    PubMed

    Krizkova, Sona; Krystofova, Olga; Trnkova, Libuse; Hubalek, Jaromir; Adam, Vojtech; Beklova, Miroslava; Horna, Ales; Havel, Ladislav; Kizek, Rene

    2009-01-01

    We used carbon paste electrodes and a standard potentiostat to detect silver ions. The detection limit (3 Signal/Noise ratio) was estimated as 0.5 μM. A standard electrochemical instrument microanalysis of silver(I) ions was suggested. As a working electrode a carbon tip (1 mL) or carbon pencil was used. Limits of detection estimated by dilution of a standard were 1 (carbon tip) or 10 nM (carbon pencil). Further we employed flow injection analysis coupled with carbon tip to detect silver(I) ions released in various beverages and mineral waters. During first, second and third week the amount of silver(I) ions releasing into water samples was under the detection limit of the technique used for their quantification. At the end of a thirteen weeks long experiment the content of silver(I) ions was several times higher compared to the beginning of release detected in the third week and was on the order of tens of nanomoles. In subsequent experiments the influence of silver(I) ions (0, 5 and 10 μM) on a plant model system (tobacco BY-2 cells) during a four-day exposition was investigated. Silver(I) ions were highly toxic to the cells, which was revealed by a double staining viability assay. Moreover we investigated the effect of silver(I) ions (0, 0.3, 0.6, 1.2 and 2.5 μM) on guppies (Poecilia reticulata). Content of Ag(I) increased with increasing time of the treatment and applied concentrations in fish tissues. It can be concluded that a carbon tip or carbon pencil coupled with a miniaturized potentiostat can be used for detection of silver(I) ions in environmental samples and thus represents a small, portable, low cost and easy-to-use instrument for such purposes. PMID:22399980

  1. Silver(I) Ions Ultrasensitive Detection at Carbon Electrodes—Analysis of Waters, Tobacco Cells and Fish Tissues

    PubMed Central

    Krizkova, Sona; Krystofova, Olga; Trnkova, Libuse; Hubalek, Jaromir; Adam, Vojtech; Beklova, Miroslava; Horna, Ales; Havel, Ladislav; Kizek, Rene

    2009-01-01

    We used carbon paste electrodes and a standard potentiostat to detect silver ions. The detection limit (3 Signal/Noise ratio) was estimated as 0.5 μM. A standard electrochemical instrument microanalysis of silver(I) ions was suggested. As a working electrode a carbon tip (1 mL) or carbon pencil was used. Limits of detection estimated by dilution of a standard were 1 (carbon tip) or 10 nM (carbon pencil). Further we employed flow injection analysis coupled with carbon tip to detect silver(I) ions released in various beverages and mineral waters. During first, second and third week the amount of silver(I) ions releasing into water samples was under the detection limit of the technique used for their quantification. At the end of a thirteen weeks long experiment the content of silver(I) ions was several times higher compared to the beginning of release detected in the third week and was on the order of tens of nanomoles. In subsequent experiments the influence of silver(I) ions (0, 5 and 10 μM) on a plant model system (tobacco BY-2 cells) during a four-day exposition was investigated. Silver(I) ions were highly toxic to the cells, which was revealed by a double staining viability assay. Moreover we investigated the effect of silver(I) ions (0, 0.3, 0.6, 1.2 and 2.5 μM) on guppies (Poecilia reticulata). Content of Ag(I) increased with increasing time of the treatment and applied concentrations in fish tissues. It can be concluded that a carbon tip or carbon pencil coupled with a miniaturized potentiostat can be used for detection of silver(I) ions in environmental samples and thus represents a small, portable, low cost and easy-to-use instrument for such purposes. PMID:22399980

  2. A XPS Study of the Passivity of Stainless Steels Influenced by Sulfate-Reducing Bacteria.

    NASA Astrophysics Data System (ADS)

    Chen, Guocun

    The influence of sulfate-reducing bacteria (SRB) on the passivity of type 304 and 317L stainless steels (SS) was investigated by x-ray photoelectron spectroscopy (XPS), microbiological and electrochemical techniques. Samples were exposed to SRB, and then the resultant surfaces were analyzed by XPS, and the corrosion resistance by potentiodynamic polarization in deaerated 0.1 M HCl. To further understand their passivity, the SRB-exposed samples were analyzed by XPS after potentiostatic polarization at a passive potential in the hydrochloric solution. The characterization was performed under two surface conditions: unrinsed and rinsed by deaerated alcohol and deionized water. Comparisons were made with control samples immersed in uninoculated medium. SRB caused a severe loss of the passivity of 304 SS through sulfide formation and possible additional activation to form hexavalent chromium. The sulfides included FeS, FeS_2, Cr_2S _3, NiS and possibly Fe_ {rm 1-x}S. The interaction took place nonuniformly, resulting in undercutting of the passive film and preferential hydration of inner surface layers. The bacterial activation of the Cr^{6+ }^ecies was magnified by subsequent potentiostatic polarization. In contrast, 317L SS exhibited a limited passivity. The sulfides were formed mainly in the outer layers. Although Cr^{6+}^ecies were observed after the exposure, they were dissolved upon polarization. Since 317L SS has a higher Mo content, its higher passivity was ascribed to Mo existing as molybdate on the surface and Mo^{5+} species in the biofilm. Consequently, the interaction of SRB with Mo was studied. It was observed that molybdate could be retained on the surfaces of Mo coupons by corrosion products. In the presence of SRB, however, a considerable portion of the molybdate interacted with intermediate sulfur -containing proteins, forming Mo(V)-S complexes and reducing bacterial growth and sulfate reduction. The limited insolubility of the Mo(V)-S complexes in 0.1 M HCl provided a certain protection so that the pitting potential of the SRB-exposed Mo coupons was not considerably decreased. The interaction of the sulfur-containing proteins with Mo also provided mechanistic information about the adhesion of biofilm to Mo-bearing steels. Additionally, the interactions of SRB with other alloying elements, Cr and Ni, were investigated.

  3. Design, Fabrication, and Characterization of Organic Electronic Devices for Thermoelectric Applications

    NASA Astrophysics Data System (ADS)

    Yablonski, Joshua David

    Thermoelectric devices are an emerging application for conducting organic materials. Translating between heat and electricity, these materials could help to meet the energy needs of the future. Organic materials are advantageous because of their flexibility, processability, low toxicity, and cost. However, organic thermoelectric devices are presently lower efficiency than their inorganic counterparts, due to their lower electrical conductivities. This work seeks to progress towards higher-efficiency organic thermoelectric devices using several different approaches. First, poly(3,4-ethylenedioxythiophene) (PEDOT) thin-films were polymerized electrochemically onto a surface using galvanostatic, potentiostatic, and potentiodynamic techniques. It was determined that the surface morphologies of the potentiostatic and galvanostatic films are quite similar, but the potentiodynamic morphology is markedly different. An electrochemical dedoping process was developed for these films, and the degree of dedoping was monitored with UV-Vis and XPS. The oxidation levels in the films were found to vary between 11.7 and 33%. The electrical conductivity, Seebeck coefficient, and thermoelectric power factor of the PEDOT films were measured, and a maximum value of 13.6 microW m-1 K-2 was obtained. Second, two analogous polymers, HTAZ and FTAZ, were studied for future thermoelectric use. The polymers were chemically doped with FeCl3, the degree of doping was monitored with UV-Vis, and the doping stabilities of both polymers were recorded. The electrical conductivity was also measured and related to the doping level. Despite the space-charge limited current (SCLC) mobility of FTAZ being nearly an order of magnitude higher than HTAZ, the conductivities were nearly identical. Finally, as a way to increase mobility and conductivity in future organic thermoelectric devices, a novel metal-molecule-metal junction was designed and fabricated using an adapted transfer-printing technique. Patterned gold contacts were transferred onto poly(3-methylthiophene) (P3MT) brushes anchored to an ITO electrode. The junctions were electrically characterized via conducting AFM to determine charge transport behavior, and the SCLC mobility was extracted from the current-voltage curves. The polymer brush devices could be improved by annealing before transfer of the top gold contacts, and this led to a maximum increase of two orders of magnitude in device mobility.

  4. Utilization of subsurface microbial electrochemical systems to elucidate the mechanisms of competition between methanogenesis and microbial iron(III)/humic acid reduction in Arctic peat soils

    NASA Astrophysics Data System (ADS)

    Friedman, E. S.; Miller, K.; Lipson, D.; Angenent, L. T.

    2012-12-01

    High-latitude peat soils are a major carbon reservoir, and there is growing concern that previously dormant carbon from this reservoir could be released to the atmosphere as a result of continued climate change. Microbial processes, such as methanogenesis and carbon dioxide production via iron(III) or humic acid reduction, are at the heart of the carbon cycle in Arctic peat soils [1]. A deeper understanding of the factors governing microbial dominance in these soils is crucial for predicting the effects of continued climate change. In previous years, we have demonstrated the viability of a potentiostatically-controlled subsurface microbial electrochemical system-based biosensor that measures microbial respiration via exocellular electron transfer [2]. This system utilizes a graphite working electrode poised at 0.1 V NHE to mimic ferric iron and humic acid compounds. Microbes that would normally utilize these compounds as electron acceptors donate electrons to the electrode instead. The resulting current is a measure of microbial respiration with the electrode and is recorded with respect to time. Here, we examine the mechanistic relationship between methanogenesis and iron(III)- or humic acid-reduction by using these same microbial-three electrode systems to provide an inexhaustible source of alternate electron acceptor to microbes in these soils. Chamber-based carbon dioxide and methane fluxes were measured from soil collars with and without microbial three-electrode systems over a period of four weeks. In addition, in some collars we simulated increased fermentation by applying acetate treatments to understand possible effects of continued climate change on microbial processes in these carbon-rich soils. The results from this work aim to increase our fundamental understanding of competition between electron acceptors, and will provide valuable data for climate modeling scenarios. 1. Lipson, D.A., et al., Reduction of iron (III) and humic substances plays a major role in anaerobic respiration in an Arctic peat soil. Journal of Geophysical Research-Biogeosciences, 2010. 115. 2. Friedman, E.S., et al., A cost-effective and field-ready potentiostat that poises subsurface electrodes to monitor bacterial respiration. Biosensors and Bioelectronics, 2012. 32(1): p. 309-313.

  5. Triboelectrochemical characterization of microelectronic materials

    NASA Astrophysics Data System (ADS)

    Joo, Suk Bae

    Non-uniformity in chemical-mechanical planarization (CMP) due to diverse pattern geometry in copper damascene structures has been a critical limit to process yield. Fundamental understanding in tribology and electrochemistry is crucial to solve this problem. This research develops novel triboelectrochemical techniques to characterize the polished wafer surface and to understand mechanisms of materials removal. There are two approaches in this research. Experimentally, a setup containing a tribometer and a potentiostat was built. It enabled simultaneous measurement in friction coefficient and electrochemical response of wafer materials. Theoretically, electrochemical reactions and Hertzian contact were analyzed on ECMPed wafers in terms of mechanisms of step height reduction in anodic and cathodic ECMP in corresponds to surface chemistry. Results revealed the nature of limitation of ECMP for global planarization. In order to further the fundamental investigation of ECMP, the potentiostatic electrochemical impedance spectroscopy (EIS) was utilized to study the interface kinetics. It was revealed that the formation of Cu oxide films was affected by the electrical potentials. Through in situ measurement, it was found that the tribological behavior depend on the surface chemistry and surface morphology under the influence of anodic potentials. The potentiodynamic polarization results explained the removal and formation mechanisms of interface. The results showed that the cycle of passivation/removal was a function of mechanical factor such as the load and speed. The new model was developed via material removal rate (MRR) in both electrochemical and mechanical aspects. The quantitative contribution of iii electrochemical potential to overall removal was established for the first time. It was further confirmed by Ru and the electrochemical constant j was developed for metal ECMP. This dissertation includes seven chapters. Chapter I Introduction and II Motivation and Objectives are followed by the materials setup and testing conditions discussed in Chapter III. The tribological and electrochemical characterization of the Cu patterned geometry is discussed in Chapter IV. Chapter V discusses the kinetics of the interface during polishing and its removal mechanisms. Chapter VI discusses the synergism of ECMP, followed by Conclusions and Future work.

  6. Deformation and fracture of aluminum-lithium alloys: The effect of dissolved hydrogen

    NASA Technical Reports Server (NTRS)

    Rivet, F. C.; Swanson, R. E.

    1990-01-01

    The effects of dissolved hydrogen on the mechanical properties of 2090 and 2219 alloys are studied. The work done during this semi-annual period consists of the hydrogen charging study and some preliminary mechanical tests. Prior to SIMS analysis, several potentiostatic and galvanostatic experiments were performed for various times (going from 10 minutes to several hours) in the cathodic zone, and for the two aqueous solutions: 0.04N of HCl and 0.1N NaOH both combined with a small amount of As2O3. A study of the surface damage was conducted in parallel with the charging experiments. Those tests were performed to choose the best charging conditions without surface damage. Disk rupture tests and tensile tests are part of the study designed to investigate the effect of temperature, surface roughness, strain rate, and environment on the fracture behavior. The importance of the roughness and environment were shown using the disk rupture test as well as the importance of the strain rate under hydrogen environment. The tensile tests, without hydrogen effects, have not shown significant differences between low and room temperature.

  7. A laminar-flow microfluidic device for quantitative analysis of microbial electrochemical activity.

    PubMed

    Li, Zhongjian; Venkataraman, Arvind; Rosenbaum, Miriam A; Angenent, Largus T

    2012-06-01

    We report a laminar flow-based microfluidic bioelectrochemical system (BES) that was fabricated by using polydimethyl siloxane (PDMS) channels and gold electrodes. The microfluidic BES was operated as a potentiostatically controlled two-electrode system. A pure culture of Geobacter sulfurreducens strain PCA, which is a model electrode-respiring bacterium, was grown in the channel and respired with the electrode under strict anaerobic conditions. We took advantage of the short hydraulic retention time (≈ 2 min) and response times (<21 min) to rapidly test the effect of certain chemical stimuli, such as O(2) and anthraquinone disulfide (AQDS), on electric current production by G. sulfurreducens. The results showed that: i) short-term (2 min) exposure to O(2) -saturated solution did not cause any irreversible toxicity to G. sulfurreducens, and ii) AQDS can be used as a redox mediator by G. sulfurreducens for shuttling electrons between the microbe and the electrode. We, therefore, demonstrate that the microfluidic BES is a promising research tool for gaining insight into microbial electrochemical activity. In our two-dimensional microfluidic-based research tool, a well-defined electrochemical environment can be maintained with the help of laminar flow without a membrane to separate two electrodes. PMID:22674693

  8. A laminar-flow microfluidic device for quantitative analysis of microbial electrochemical activity.

    TOXLINE Toxicology Bibliographic Information

    Li Z; Venkataraman A; Rosenbaum MA; Angenent LT

    2012-06-01

    We report a laminar flow-based microfluidic bioelectrochemical system (BES) that was fabricated by using polydimethyl siloxane (PDMS) channels and gold electrodes. The microfluidic BES was operated as a potentiostatically controlled two-electrode system. A pure culture of Geobacter sulfurreducens strain PCA, which is a model electrode-respiring bacterium, was grown in the channel and respired with the electrode under strict anaerobic conditions. We took advantage of the short hydraulic retention time (≈ 2 min) and response times (<21 min) to rapidly test the effect of certain chemical stimuli, such as O(2) and anthraquinone disulfide (AQDS), on electric current production by G. sulfurreducens. The results showed that: i) short-term (2 min) exposure to O(2) -saturated solution did not cause any irreversible toxicity to G. sulfurreducens, and ii) AQDS can be used as a redox mediator by G. sulfurreducens for shuttling electrons between the microbe and the electrode. We, therefore, demonstrate that the microfluidic BES is a promising research tool for gaining insight into microbial electrochemical activity. In our two-dimensional microfluidic-based research tool, a well-defined electrochemical environment can be maintained with the help of laminar flow without a membrane to separate two electrodes.

  9. Lithographically Patterned PEDOT Nanowires for the Detection of Iron(III) with Nanomolar Sensitivity.

    PubMed

    Kindra, Lindsay R; Eggers, Crystin J; Liu, Andrew T; Mendoza, Kelly; Mendoza, Jennifer; Klein Myers, Aviva R; Penner, Reginald M

    2015-11-17

    Arrays of nanowires of an electronically conductive polymeric affinity medium tailored to the detection of Fe(III) are prepared, and their properties for detecting Fe(III) are evaluated. This polymeric affinity medium consists of poly(3,4-ethylenedioxythiophene) (PEDOT) into which an iron chelator, deferoxamine (DFA), has been doped during the polymerization process. PEDOT-DFA nanowires are potentiostatically deposited from a solution containing both EDOT and DFA using lithographically patterned nanowire electrodeposition (LPNE). The through-nanowire electrical resistance of PEDOT-DFA nanowires is measured as a function of the Fe(III) concentration. In parallel with measurements on PEDOT-DFA nanowire arrays, the electrochemical impedance of PEDOT-DFA films is characterized as a function of the Fe(III) concentration and the frequency of the impedance measurement in order to better understand the mechanism of transduction. PEDOT-DFA nanowires detect Fe(III) from 10(-4) to 10(-8) M with a limit of detection of 300 pM (calculated) and 10 nM (measured). PMID:26499338

  10. Stress-corrosion behavior of aluminum-lithium alloys in aqueous salt environments

    NASA Technical Reports Server (NTRS)

    Pizzo, P. P.; Galvin, R. P.; Nelson, H. G.

    1984-01-01

    The stress corrosion susceptibility of two powder metallurgy (P/M) alloys, Al-Li-Cu and Al-Li-Cu-Mg; two mechanically attrited (M/A) alloys, Al-Li-Cu and Al-Li-Mg; and two wrought, ingot alloys, X-2020 and AA7475, are compared. Time-dependent fracture in an aqueous sodium chloride environment under alternate immersion condition was found to vary significantly between alloys. The stress corrosion behavior of the two powder metallurgy processed alloys was studied in detail under conditions of crack initiation, static crack growth, and fatigue crack growth. A variety of stress corrosion tests were performed including smooth surface, time-to-failure tests; potentiostatic tests on smooth surfaces exposed to constant applied strain rates; and fracture mechanics-type tests under static and cyclic loads. Both alloys show surface pitting and subsequent intergranular corrosion. Pitting is more severe in the magnesium-bearing alloy and is associated with stringer particles strung along the extrusion direction as a result of P/M processing.

  11. Amperometric Sensor for Detection of Chloride Ions†

    PubMed Central

    Trnkova, Libuse; Adam, Vojtech; Hubalek, Jaromir; Babula, Petr; Kizek, Rene

    2008-01-01

    Chloride ion sensing is important in many fields such as clinical diagnosis, environmental monitoring and industrial applications. We have measured chloride ions at a carbon paste electrode (CPE) and at a CPE modified with solid AgNO3, a solution of AgNO3 and/or solid silver particles. Detection limits (3 S/N) for chloride ions were 100 μM, 100 μM and 10 μM for solid AgNO3, solution of AgNO3 and/or solid silver particles, respectively. The CPE modified with silver particles is the most sensitive to the presence chloride ions. After that we approached to the miniaturization of the whole electrochemical instrument. Measurements were carried out on miniaturized instrument consisting of a potentiostat with dimensions 35 × 166 × 125 mm, screen printed electrodes, a peristaltic pump and a PC with control software. Under the most suitable experimental conditions (Britton-Robinson buffer, pH 1.8 and working electrode potential 550 mV) we estimated the limit of detection (3 S/N) as 500 nM.

  12. Hydrogen trapping in high-strength steels

    SciTech Connect

    Pound, B.G.

    1998-10-09

    Hydrogen trapping in three high-strength steels -- AerMet 100 and AISI 4340 and H11 -- was studied using a potentiostatic pulse technique. Irreversible trapping constants (k) and hydrogen entry fluxes were determined for these alloys in 1 mol/1 acetic acid/1 mol/1 sodium acetate. The order of the k values for the three steels and two 18Ni maraging steels previously studies inversely parallels their threshold stress intensities for stress corrosion cracking (K{sub 1SCC}). Irreversible trapping in AerMet 100 varies with aging temperature and appears to depend on the type of carbide (Fe{sub 3}C or M{sub 2}C) present. For 4340 steel, k can be correlated with K{sub 1SCC} over a range of yield strengths. The change in k is consistent with a change in the principal type of irreversible trap from matrix boundaries to incoherent Fe{sub 3}C. The principal irreversible traps in H11 at high yield strengths are thought to be similar to those in 4340 steel.

  13. Batch-injection analysis with amperometric detection of the DPPH radical for evaluation of antioxidant capacity.

    PubMed

    Oliveira, Gracy K F; Tormin, Thiago F; Sousa, Raquel M F; de Oliveira, Alberto; de Morais, Sérgio A L; Richter, Eduardo M; Munoz, Rodrigo A A

    2016-02-01

    This work proposes the application of batch-injection analysis with amperometric detection to determine the antioxidant capacity of real samples based on the measurement of DPPH radical consumption. The efficient concentration or EC50 value corresponds to the concentration of sample or standard required to scavenge 50% DPPH radicals. For the accurate determination of EC50, samples were incubated with DPPH radical for 1h because many polyphenolic compounds typically found in plants and responsible for the antioxidant activity exhibit slow kinetics. The BIA system with amperometric detection using a glassy-carbon electrode presented high precision (RSD = 0.7%, n = 12), low detection limit (1 μmol L(-1)) and selective detection of DPPH (free of interferences from antioxidants). These contributed to low detection limits for the antioxidant (0.015 and 0.19 μmol L(-1) for gallic acid and butylated hydroxytoluene, respectively). Moreover, BIA methods show great promise for portable analysis because battery-powered instrumentation (electronic micropipette and potentiostats) is commercially available. PMID:26304399

  14. In vitro biocorrosion of Co-Cr-Mo implant alloy by macrophage cells.

    PubMed

    Lin, Hsin-Yi; Bumgardner, Joel D

    2004-11-01

    We hypothesized that macrophage cells and their released reactive chemical species (RCS) affect Co-Cr-Mo alloy's corrosion properties and that alloy corrosion products change macrophage cell behavior. A custom cell culture corrosion cell was used to evaluate how culture medium, cells, and RCS altered alloy corrosion in 3-day tests. Corrosion was evaluated by measuring total charge transfer at a constant potential using a potentiostat and metal ion release by atomic emission spectroscopy. Viability, proliferation, and NO (nitric oxide) and IL-1beta (interlukin-1beta) release were used to assess cellular response to alloy corrosion products. In the presence of activated cells, total charge transfers and Co ion release were the lowest (p < 0.05). This was attributed to an enhancement of the surface oxide by RCS. Cr and Mo release were not different between cells and activated cells. Low levels of metal ions did not affect cell viability, proliferation, or NO release, though IL-1beta released from the activated cells was higher on the alloy compared to the controls. These data support the hypothesis that macrophage cells and their RCS affect alloy corrosion. Changes in alloy corrosion by cells may be important to the development of host responses to the alloy and its corrosion products. PMID:15475202

  15. Influence of the sliding velocity and the applied potential on the corrosion and wear behavior of HC CoCrMo biomedical alloy in simulated body fluids.

    PubMed

    Gil, Roberto Alonso; Muñoz, Anna Igual

    2011-11-01

    The corrosion and tribocorrosion behavior of an as-cast high carbon CoCrMo alloy immersed in phosphate buffered solution (PBS) and phosphate buffered solution with bovine serum albumin (PBS+BSA) have been analyzed by electrochemical techniques and surface microscopy. After the electrochemical characterization of the alloy in both solutions, the sample was studied tribo-electrochemically (by open circuit potential, OCP measurements, potentiodynamic curves and potentiostatic tests) in a ball-on-disk tribometer rotating in different sliding velocities. The influence of solution chemistry, sliding velocity and applied potential on the corrosion and tribocorrosion behavior of the CoCrMo alloy has been studied. Anodic current density increases with sliding velocity but wear rate does not change at an applied anodic potential; on the other hand, BSA modifies the wear debris behavior (by agglomerating the debris formed by mechanical removal of particles) thus increasing the mechanical wear volume. Under cathodic conditions, cathodic current density also increases during mechanical contact while the wear rate decreases with sliding velocity and BSA lubricates the contact thus reducing the total wear volume with respect to the non-containing BSA solution. The work shows how the electrode potential critically affects the corrosion and tribocorrosion rates by increasing the wear coefficients at applied anodic potentials due to severe wear accelerated corrosion. PMID:22098909

  16. Electrochemical characteristics of a carbon fibre composite and the associated galvanic effects with aluminium alloys

    NASA Astrophysics Data System (ADS)

    Liu, Z.; Curioni, M.; Jamshidi, P.; Walker, A.; Prengnell, P.; Thompson, G. E.; Skeldon, P.

    2014-09-01

    The electrochemical behaviour of a carbon fibre reinforced epoxy matrix composite in 3.5% NaCl and 3.5% NaCl + 0.5 M CuSO4 electrolytes was examined by potentiodynamic polarisation, potentiostatic polarisation and scanning electron microscopy. Exposed carbon fibres on two defined regions (“front” and “side”) are a focus of the investigation. The large size of the exposed carbon fibres on the side region is responsible for a higher cathodic current density than the front region in the NaCl electrolyte. The deposition of copper on the front surface of composite confirmed that the significantly higher cathodic current resulted from the exposure of the fibres to the NaCl electrolyte. Galvanic coupling between the composite and individual aluminium alloys (AA7075-T6 and AA1050) was used to measure galvanic potentials and galvanic current densities. The highly alloyed AA7075-T6 alloy and its high population density of cathodic sites compared to the AA1050 acted to reduce the galvanic effect when coupled to the composite front or side regions.

  17. Dissolution and corrosion inhibition of copper, zinc, and their alloys

    SciTech Connect

    Jinturkar, P.; Guan, Y.C.; Han, K.N.

    1998-02-01

    The corrosion behavior of copper, zinc, and their alloys in sulfuric acid (H{sub 2}SO{sub 4}) solutions with oxygen and ferric ions (Fe{sup 3+}) was studied using a potentiostat. Oxygen and Fe{sup 3+} ions were shown to play an important role in corrosion of copper and copper-zinc alloys. Cathodic reduction of oxygen mainly was controlled by chemical reaction, and that of Fe{sup 3+} ions was controlled by diffusion. The overall cathodic process was the summation of the reduction of oxygen and Fe{sup 3+} ions. Corrosion of zinc was controlled mainly by reduction of water. Corrosion inhibition using benzotriazole (BTAH) also was investigated in aerated and deaerated solutions. BTAH was found to be a useful inhibitor, and the inhibition layer was shown to be stable and persistent. Morphology of the surface of copper, zinc, and brasses after corrosion in the presence and absence of BTAH was examined by scanning electron microscopy. BTAH formed a protective layer on the surface, thereby inhibiting corrosion. Solution analysis of the dissolution of brasses showed that zinc dissolved preferentially in the initial stages, followed by simultaneous dissolution of copper and zinc.

  18. A reusable capacitive immunosensor based on a CuS ultrathin film constructed by using a surface sol-gel technique.

    PubMed

    Wu, Zhan; Cao, Zhong; Zeng, Ju-Lan; Zhang, Ling; Chu, Xia; Shen, Guo-Li; Yu, Ru-Qin

    2010-01-01

    A capacitive sensing method based on a CuS ultrathin film modified electrode prepared by a surface sol-gel technique has been developed for the direct detection of human IgA. The resulting CuS film was investigated with cyclic voltammetry (CV), impedance spectroscopy, and quartz crystal microbalance (QCM). CV and impedance examinations showed that the CuS film formed on the gold electrode surface was insulated, and was applicable to form an insulating layer of a capacitive immunosensor. With QCM measurements, the thickness of the CuS film was evaluated to be 5.8 nm. The capacitance change was greatly increased by a CuS nanofilm-based immunosensor, which was initiated by the recognition of an immobilized antibody and the target antigen. The capacitance of the immunosensor corresponding to the concentration of human IgA was investigated by potentiostatic-step measurements. A linear calibration curve was obtained in the range of 1.81 - 90.5 ng ml(-1) with a detection limit of 1.81 ng ml(-1). There were no obvious interferences from the nonspecific adsorption of other proteins. With nice reproducibility and regeneration capacity, the CuS ultrathin film modified immunosensor could be used for the detection of human IgA in serum samples with a recovery of 96.1 - 104.4%, showing its promising applicability and reliability. PMID:20834134

  19. Electrochemical study of resistance to localized corrosion of stainless steels for biomaterial applications

    SciTech Connect

    Pan, J.; Karlen, C.; Ulfvin, C.

    2000-03-01

    Sandvik Bioline High-N and 316 LVM are two austenitic stainless steels especially developed for biomaterial applications. Their resistance to localized corrosion was investigated by electrochemical methods including cyclic potentiodynamic polarization and potentiostatic polarization measurements in a phosphate-buffered saline solution and in a simulated crevice solution, i.e., designed for crevice corrosion testing. Sandvik SAF 2507 (a high-performance super duplex stainless steel) was included in the tests as a reference material High-N, higher alloyed than 316 LVM, demonstrated excellent resistance to pitting initiation and a strong tendency to repassivation. High-N proved to have an equivalent or even higher resistance to localized corrosion than SAF 2507. The latter is known for its impressive corrosion properties, particularly in chloride containing environments. While 316 LVM may run the risk of crevice corrosion in implant applications, the risk seems negligible for High-N. In view of the fact that also the mechanical properties are superior to those of 316 LVM, High-N is a very attractive implant material.

  20. An in vitro investigation of the anodic polarization and capacitance behavior of 316-L stainless steel.

    PubMed

    Sutow, E J; Pollack, S R; Korostoff, E

    1976-09-01

    Determinations were made of how the corrosion-resistant properties of the passive film on 316-L stainless steel are influenced by the material's mechanical and surface states, and the variable pH and PO2 conditions of the interstitial fluid. Cold-rolled and annealed specimens were surface-prepared, commercially and in the laboratory, respectively, as if for orthopedic implantation. Passive film behavior was studied by the anodic polarization and pulse-potentiostatic capacitance methods. The pH and PO2 of the Ringer's test solution were varied to include interstitial fluid values occurring postoperatively and onto recovery. The anodic polarization behavior of all specimens was found to be pH- and PO2-independent. Breakdown potentials of annealed specimens were 800-950 mV (SCE), in contrast to previously reported values of approximately 350 mV. This substantial increase is related to the influence of surface preparation and, in particular, to the optimization of electropolishing time which acts to produce a microscopically smooth surface, free of debris and disarrayed material. Capacitance behavior of annealed material for potentials greater than 400 mV was consistent with a model involving the entry of chloride and metal ions (mostly Fe) into the passive film. This entry is related to the onset of pitting. PMID:10307

  1. The effect of additives on the nucleation and growth of copper onto stainless steel cathodes

    NASA Astrophysics Data System (ADS)

    Sun, M.; O'Keefe, T. J.

    1992-10-01

    A potentiostatic technique has been used to study the effects of chloride ion, glue, and thiourea on the initial electrodeposition of copper. A stainless steel (AISI 304) rotating disc electrode (RDE) with an electrolyte containing 40 g/1 Cu2+ and 180 g/1 H2SO4 at 40 °C was employed. The current transients from the potential step measurements for the additive-free electrolyte could be fitted to a model that assumed progressive nucleation followed by growth of three-dimensional (3-D) centers under diffusion control. The growth mechanism and the type of nuclei were also confirmed by scanning electron microscopy (SEM) of the deposit. Chloride ions (40 ppm) affect the rate of the reaction, decrease the number of nuclei, and enhance the growth process. The particular glue (TPC 69, 5 ppm) used in this work is a polarizer and increases the number of nuclei formed on the surface. For the experimental parameters used in this research, the nucleation and growth mechanism is not changed by the presence of chloride ion or glue in the electrolyte. However, thiourea (0.5 ppm) additions caused the mechanism to change to instantaneous nucleation with 3-D growth under kinetic control, and a large number of equal sized nuclei are observed on the SEM micrographs, tending to verify the proposed mechanism.

  2. Ultrafast charge separation dynamics in opaque, operational dye-sensitized solar cells revealed by femtosecond diffuse reflectance spectroscopy

    NASA Astrophysics Data System (ADS)

    Ghadiri, Elham; Zakeeruddin, Shaik M.; Hagfeldt, Anders; Grätzel, Michael; Moser, Jacques-E.

    2016-04-01

    Efficient dye-sensitized solar cells are based on highly diffusive mesoscopic layers that render these devices opaque and unsuitable for ultrafast transient absorption spectroscopy measurements in transmission mode. We developed a novel sub-200 femtosecond time-resolved diffuse reflectance spectroscopy scheme combined with potentiostatic control to study various solar cells in fully operational condition. We studied performance optimized devices based on liquid redox electrolytes and opaque TiO2 films, as well as other morphologies, such as TiO2 fibers and nanotubes. Charge injection from the Z907 dye in all TiO2 morphologies was observed to take place in the sub-200 fs time scale. The kinetics of electron-hole back recombination has features in the picosecond to nanosecond time scale. This observation is significantly different from what was reported in the literature where the electron-hole back recombination for transparent films of small particles is generally accepted to occur on a longer time scale of microseconds. The kinetics of the ultrafast electron injection remained unchanged for voltages between +500 mV and –690 mV, where the injection yield eventually drops steeply. The primary charge separation in Y123 organic dye based devices was clearly slower occurring in two picoseconds and no kinetic component on the shorter femtosecond time scale was recorded.

  3. Ultrafast charge separation dynamics in opaque, operational dye-sensitized solar cells revealed by femtosecond diffuse reflectance spectroscopy.

    PubMed

    Ghadiri, Elham; Zakeeruddin, Shaik M; Hagfeldt, Anders; Grätzel, Michael; Moser, Jacques-E

    2016-01-01

    Efficient dye-sensitized solar cells are based on highly diffusive mesoscopic layers that render these devices opaque and unsuitable for ultrafast transient absorption spectroscopy measurements in transmission mode. We developed a novel sub-200 femtosecond time-resolved diffuse reflectance spectroscopy scheme combined with potentiostatic control to study various solar cells in fully operational condition. We studied performance optimized devices based on liquid redox electrolytes and opaque TiO2 films, as well as other morphologies, such as TiO2 fibers and nanotubes. Charge injection from the Z907 dye in all TiO2 morphologies was observed to take place in the sub-200 fs time scale. The kinetics of electron-hole back recombination has features in the picosecond to nanosecond time scale. This observation is significantly different from what was reported in the literature where the electron-hole back recombination for transparent films of small particles is generally accepted to occur on a longer time scale of microseconds. The kinetics of the ultrafast electron injection remained unchanged for voltages between +500 mV and -690 mV, where the injection yield eventually drops steeply. The primary charge separation in Y123 organic dye based devices was clearly slower occurring in two picoseconds and no kinetic component on the shorter femtosecond time scale was recorded. PMID:27095505

  4. An Implantable RFID Sensor Tag toward Continuous Glucose Monitoring.

    PubMed

    Xiao, Zhibin; Tan, Xi; Chen, Xianliang; Chen, Sizheng; Zhang, Zijian; Zhang, Hualei; Wang, Junyu; Huang, Yue; Zhang, Peng; Zheng, Lirong; Min, Hao

    2015-05-01

    This paper presents a wirelessly powered implantable electrochemical sensor tag for continuous blood glucose monitoring. The system is remotely powered by a 13.56-MHz inductive link and utilizes an ISO 15693 radio frequency identification (RFID) standard for communication. This paper provides reliable and accurate measurement for changing glucose level. The sensor tag employs a long-term glucose sensor, a winding ferrite antenna, an RFID front-end, a potentiostat, a 10-bit sigma-delta analog to digital converter, an on-chip temperature sensor, and a digital baseband for protocol processing and control. A high-frequency external reader is used to power, command, and configure the sensor tag. The only off-chip support circuitry required is a tuned antenna and a glucose microsensor. The integrated chip fabricated in SMIC 0.13-μm CMOS process occupies an area of 1.2 mm ×2 mm and consumes 50 μW. The power sensitivity of the whole system is -4 dBm. The sensor tag achieves a measured glucose range of 0-30 mM with a sensitivity of 0.75 nA/mM. PMID:25823049

  5. Wearable salivary uric acid mouthguard biosensor with integrated wireless electronics.

    PubMed

    Kim, Jayoung; Imani, Somayeh; de Araujo, William R; Warchall, Julian; Valdés-Ramírez, Gabriela; Paixão, Thiago R L C; Mercier, Patrick P; Wang, Joseph

    2015-12-15

    This article demonstrates an instrumented mouthguard capable of non-invasively monitoring salivary uric acid (SUA) levels. The enzyme (uricase)-modified screen printed electrode system has been integrated onto a mouthguard platform along with anatomically-miniaturized instrumentation electronics featuring a potentiostat, microcontroller, and a Bluetooth Low Energy (BLE) transceiver. Unlike RFID-based biosensing systems, which require large proximal power sources, the developed platform enables real-time wireless transmission of the sensed information to standard smartphones, laptops, and other consumer electronics for on-demand processing, diagnostics, or storage. The mouthguard biosensor system offers high sensitivity, selectivity, and stability towards uric acid detection in human saliva, covering the concentration ranges for both healthy people and hyperuricemia patients. The new wireless mouthguard biosensor system is able to monitor SUA level in real-time and continuous fashion, and can be readily expanded to an array of sensors for different analytes to enable an attractive wearable monitoring system for diverse health and fitness applications. PMID:26276541

  6. Ion and gas chromatography mass spectrometry investigations of organophosphates in lithium ion battery electrolytes by electrochemical aging at elevated cathode potentials

    NASA Astrophysics Data System (ADS)

    Weber, Waldemar; Wagner, Ralf; Streipert, Benjamin; Kraft, Vadim; Winter, Martin; Nowak, Sascha

    2016-02-01

    The electrochemical aging of commercial non-aqueous lithium hexafluorophosphate (LiPF6)/organic carbonate solvent based lithium ion battery electrolyte has been investigated in view of the formation of ionic and non-ionic alkylated phosphates. Subject was a solvent mixture of ethylene carbonate/ethyl methyl carbonate EC:EMC (1:1, by wt.) with 1 M LiPF6 (LP50 Selectilyte™, BASF). The analysis was carried out by ion chromatography coupled with electrospray ionization mass spectrometry (ESI-MS) for ionic compounds and (headspace) gas chromatography mass spectrometry ((HS)-GC-MS) for non-ionic compounds. The electrochemical aging was performed by galvanostatic charge/discharge cycling and potentiostatic experiments with LiNi0.5Mn1.5O4 (LMNO) as cathode material at increased cut-off potentials (>4.5 V vs. Li/Li+). A strong dependence of the formation of organophosphates on the applied electrode potential was observed and investigated by quantitative analysis of the formed phosphates. In addition, new possible "fingerprint" compounds for describing the electrolyte status were investigated and compared to existing compounds.

  7. Automated analysis of food-borne pathogens using a novel microbial cell culture, sensing and classification system.

    PubMed

    Xiang, Kun; Li, Yinglei; Ford, William; Land, Walker; Schaffer, J David; Congdon, Robert; Zhang, Jing; Sadik, Omowunmi

    2016-02-01

    We hereby report the design and implementation of an Autonomous Microbial Cell Culture and Classification (AMC(3)) system for rapid detection of food pathogens. Traditional food testing methods require multistep procedures and long incubation period, and are thus prone to human error. AMC(3) introduces a "one click approach" to the detection and classification of pathogenic bacteria. Once the cultured materials are prepared, all operations are automatic. AMC(3) is an integrated sensor array platform in a microbial fuel cell system composed of a multi-potentiostat, an automated data collection system (Python program, Yocto Maxi-coupler electromechanical relay module) and a powerful classification program. The classification scheme consists of Probabilistic Neural Network (PNN), Support Vector Machines (SVM) and General Regression Neural Network (GRNN) oracle-based system. Differential Pulse Voltammetry (DPV) is performed on standard samples or unknown samples. Then, using preset feature extractions and quality control, accepted data are analyzed by the intelligent classification system. In a typical use, thirty-two extracted features were analyzed to correctly classify the following pathogens: Escherichia coli ATCC#25922, Escherichia coli ATCC#11775, and Staphylococcus epidermidis ATCC#12228. 85.4% accuracy range was recorded for unknown samples, and within a shorter time period than the industry standard of 24 hours. PMID:26818563

  8. Study of the magnetization behavior of ferromagnetic nanowire array: Existence of growth defects revealed by micromagnetic simulations

    NASA Astrophysics Data System (ADS)

    Nguyen Vien, G.; Rioual, S.; Gloaguen, F.; Rouvellou, B.; Lescop, B.

    2016-03-01

    High aspect ratio nanowires were electrodeposited in nanoporous anodic alumina template by a potentiostatic method. The angular dependence of the coercive field and remanence magnetization extracted from magnetometry measurements are compared with micromagnetic simulations. Inclusion of magnetostatic interactions between Ni nanowires in simulations is required to explain some of the properties of the magnetization reversal. However, it is not sufficient to reproduce fully the angular dependence of the coercive field. Due to the polycrystalline nature of nanowires and thus to the presence of grain boundaries, defects are included in simulations. A good agreement between theory and experiment is then clearly highlighted, in particular in the nanowire easy axis direction. The achieved results allow a description of several experimental data published in the literature and consequently to get a better understanding of reversal mechanisms that operate in such nanowire arrays. A complementary study of composite nanowire array is successfully performed to prove the adequacy of the simulations method to describe the magnetic properties of nanowire array.

  9. Time-domain fitting of battery electrochemical impedance models

    NASA Astrophysics Data System (ADS)

    Alavi, S. M. M.; Birkl, C. R.; Howey, D. A.

    2015-08-01

    Electrochemical impedance spectroscopy (EIS) is an effective technique for diagnosing the behaviour of electrochemical devices such as batteries and fuel cells, usually by fitting data to an equivalent circuit model (ECM). The common approach in the laboratory is to measure the impedance spectrum of a cell in the frequency domain using a single sine sweep signal, then fit the ECM parameters in the frequency domain. This paper focuses instead on estimation of the ECM parameters directly from time-domain data. This may be advantageous for parameter estimation in practical applications such as automotive systems including battery-powered vehicles, where the data may be heavily corrupted by noise. The proposed methodology is based on the simplified refined instrumental variable for continuous-time fractional systems method ('srivcf'), provided by the Crone toolbox [1,2], combined with gradient-based optimisation to estimate the order of the fractional term in the ECM. The approach was tested first on synthetic data and then on real data measured from a 26650 lithium-ion iron phosphate cell with low-cost equipment. The resulting Nyquist plots from the time-domain fitted models match the impedance spectrum closely (much more accurately than when a Randles model is assumed), and the fitted parameters as separately determined through a laboratory potentiostat with frequency domain fitting match to within 13%.

  10. Voltage-induced morphological modifications in oocyte membranes containing exogenous K+ channels studied by electrochemical scanning force microscopy.

    PubMed

    Alessandrini, Andrea; Gavazzo, Paola; Picco, Cristiana; Facci, Paolo

    2008-04-01

    We report on a novel use of electrochemical scanning force microscopy (SFM) for the investigation of morphological modifications occurring in plasma membranes containing voltage-gated ion channels, on membrane potential variation. Membrane patches of Xenopus laevis oocytes microinjected with exogenous KAT1 cRNA, deposited by a stripping method at the surface of a derivatized gold film in inside-out configuration, have been imaged by SFM in an electrochemical cell. A potentiostat was used to maintain a desired potential drop across the membrane. Performing imaging at potential values corresponding to open (-120 mV) and closed (+20 mV) states for KAT1, morphological differences in localized sample zones were observed. Particularly, cross-shaped features involving a significant membrane portion appear around putative channel locations. The reported approach constitutes the first demonstration of an SPM-based experimental technique suitable to investigate the rearrangements occurring to the plasma membrane containing voltage-gated channels on transmembrane potential variation. PMID:18058826

  11. Understanding the fundamentals of redox mediators in Li-O2 batteries: a case study on nitroxides.

    PubMed

    Bergner, Benjamin J; Hofmann, Christine; Schürmann, Adrian; Schröder, Daniel; Peppler, Klaus; Schreiner, Peter R; Janek, Jürgen

    2015-12-21

    The development of aprotic lithium-oxygen (Li-O2) batteries suffers from high charging overvoltages. Dissolved redox mediators, like nitroxides, providing increased energy efficiency and longer lifetime are promising tools to overcome this challenge. Since this auspicious concept is still in its infancy, the underlying chemical reactions as well as the impact of the different (electro)chemical parameters are poorly understood. Herein, we derive an electrochemical model for the charging reactions, which is validated by potentiostatic measurements. The model elucidates the impact of the major factors including basic cell parameters and the chemical properties of the redox mediator. The model is applied to the promising class of nitroxides, which is systematically investigated by using derivatives of TEMPO (2,2,6,6-tetramethyl-1-piperidinyloxy), AZADO (2-azaadamantane-N-oxyl), and an azaphenalene based nitroxide. The nitroxides are electrochemically characterized by cyclic voltammetry and their performance as redox mediators is studied in Li-O2 batteries with an ether-based electrolyte. Based on the presented model, the charging profiles of the different nitroxide redox mediators are correlated with their molecular structures. PMID:26563563

  12. Entrapping cross-linked glucose oxidase aggregates within a graphitized mesoporous carbon network for enzymatic biofuel cells.

    PubMed

    Garcia-Perez, Tsai; Hong, Sung-Gil; Kim, Jungbae; Ha, Su

    2016-08-01

    This paper reports a novel method for producing glucose oxidase-nanocomposites by entrapping cross-linked glucose oxidase (GOx) aggregates within a graphitized mesoporous carbon (GMC) network. Entrapment was achieved by utilizing the strong self-aggregation tendency of GMC in aqueous buffer solution to form carbon networks. Using confocal microscopy and TEM, GOx-GMC nanocomposites were visualized. The electrochemical properties of GOx-GMC nanocomposites were studied by means of cyclic voltammograms, chronoamperometric and potentiostatic tests. Results therefrom suggested that the GOx-GMC nanocomposites offer a high electrical conductivity with the maximum electron transfer rate constant estimated at 5.16±0.61s(-1). Furthermore, thermally treating the GOx-GMC nanocomposite and GOx aggregates at 60°C for four hours, both samples maintained 99% of their initial activity, while the free GOx were completely deactivated. These performances suggested that our nanocomposite structure offered both improved electrochemical performance and stability by combining the high electrical conductivity offered by the GMC network with the high enzyme loading and stability offered by the cross-linked GOx aggregates. The GOx-GMC nanocomposite's electrochemical activity towards glucose oxidation was also investigated by using an enzymatic biofuel cell without artificial mediators, producing a power density of up to 22.4μWcm(-2) at 0.24V. PMID:27241289

  13. Mechanical performance of PPy helix tube microactuator

    NASA Astrophysics Data System (ADS)

    Bahrami Samani, Mehrdad; Spinks, Geoffrey M.; Cook, Christopher

    2004-02-01

    Conducting polymer actuators with favourable properties such as linearity, high power density and compliance are of increasing demand in micro applications. These materials generate forces over two times larger than produced by mammalian skeletal muscles. They operate to convert electro chemical energy to mechanical stress and strain. On the other hand, the application of conducting polymers is limited by the lack of a full description of the relation between four essential parameters: stress, strain, voltage and current. In this paper, polypyrrole helix tube micro actuator mechanical characteristics are investigated. The electrolyte is propylene carbonate and the dopant is TBA. PF6. The experiments are both in isotonic and isometric conditions and the input parameters are both electrical and mechanical. A dual mode force and length control and potentiostat / galvanostat are utilized for this purpose. Ultimately, the viscoelastic behaviour of the actuator is presented in this paper by a standard stress relaxation test. The effect of electrical stimulus on mechanical parameters is also explored by cyclic voltametry at different scan rates to obtain the best understanding of the actuation mechanism. The results demonstrate that the linear viscoelastic model, which performed well on conducting polymer film actuators, has to be modified to explain the mechanical behaviour of PPy helix tube fibre micro actuators. Secondly, the changes in mechanical properties of PPy need to be considered when modelling electromechanical behaviour.

  14. Construction of amperometric uric acid biosensor based on uricase immobilized on PBNPs/cMWCNT/PANI/Au composite.

    PubMed

    Rawal, Rachna; Chawla, Sheetal; Chauhan, Nidhi; Dahiya, Tulika; Pundir, C S

    2012-01-01

    A chitosan-glutaraldehyde crosslinked uricase was immobilized onto Prussian blue nanoparticles (PBNPs) absorbed onto carboxylated multiwalled carbon nanotube (c-MWCNT) and polyaniline (PANI) layer, electrochemically deposited on the surface of Au electrode. The nanohybrid-uricase electrode was characterized by scanning electron microscopic (SEM), Fourier transform infrared spectroscopy (FTIR) and cyclic voltammetry. An amperometric uric acid biosensor was fabricated using uricase/c-MWCNT/PBNPs/Au electrode as working electrode, Ag/AgCl as standard and Pt wire as auxiliary electrode connected through a potentiostat. The biosensor showed optimum response within 4s at pH 7.5 and 40°C, when operated at 0.4V vs. Ag/AgCl. The linear working range for uric acid was 0.005-0.8 mM, with a detection limit of 5 μM. The sensor was evaluated with 96% recovery of added uric acid in sera and 4.6 and 5.4% within and between batch of coefficient of variation respectively and a good correlation (r=0.99) with standard enzymic colorimetric method. This sensor measured uric acid in real serum samples. The sensor lost only 37% of its initial activity after its 400 uses over a period of 7 months, when stored at 4°C. PMID:22020190

  15. Corrosion and Fretting Corrosion Studies of Medical Grade CoCrMo Alloy in a Clinically Relevant Simulated Body Fluid Environment

    NASA Astrophysics Data System (ADS)

    Ocran, Emmanuel K.; Guenther, Leah E.; Brandt, Jan-M.; Wyss, Urs; Ojo, Olanrewaju A.

    2015-06-01

    In modular hip implants, fretting corrosion at the head/neck and neck/stem interfaces has been identified as a major cause of early revision in hip implants, particularly those with heads larger than 32 mm. It has been found that the type of fluid used to simulate the fretting corrosion of biomedical materials is crucial for the reliability of laboratory tests. Therefore, to properly understand and effectively design against fretting corrosion damage in modular hips, there is the need to replicate the human body environment as closely as possible during in vitro testing. In this work, corrosion and fretting corrosion behavior of CoCrMo in 0.14 M NaCl, phosphate buffered saline, and in a clinically relevant novel simulated body fluid was studied using a variety of electrochemical characterization techniques and tribological experiments. Electrochemical, spectroscopy and tribo-electrochemical techniques employed include Potentiodynamic polarization, Potentiostatic polarization, Electrochemical impedance spectroscopy, X-ray photoelectron spectroscopy, augur electron spectroscopy, inductively coupled plasma mass spectroscopy, and pin-on-disk wear simulation. The presence of phosphate ions in PBS accounted for the higher corrosion rate when compared with 0.14 M NaCl and the clinically relevant novel simulated body fluid. The low corrosion rates and the nature of the protective passive film formed in the clinically relevant simulated body fluid make it suitable for future corrosion and fretting corrosion studies.

  16. An electrochemical method to detect flow profiles during convection in liquid metals

    NASA Astrophysics Data System (ADS)

    Prasad, S. R.; Mallika, C.; Anderson, T. J.; Narayanan, R.

    1999-03-01

    A solid-state electrochemical method for flow visualization was developed to investigate the orientation of flow due to natural convection in semiconductor melts. The experiment was conducted in a right cylindrical ampoule made from recrystallized alumina and heated in a Bridgman furnace. Multiple solid-state electrochemical cells/sensors that were electrically insulated from one another were incorporated along the periphery of the ampoule. Liquid tin that was subject to temperature gradients was used as the model fluid to represent a high-temperature, opaque melt. Atomic oxygen was used as a tracer species, which could be potentiostatically injected or extracted locally at one of the sensors and monitored at the other cell locations on the melt/electrolyte boundaries in the galvanic mode as a function of time. Various convective flow patterns were inferred from these results for different aspect ratios of the melt and for different imposed temperature gradients. The experimental results were shown to agree qualitatively with numerical predictions.

  17. Surface, corrosion and biocompatibility aspects of Nitinol as an implant material.

    PubMed

    Shabalovskaya, Svetlana A

    2002-01-01

    The present review surveys studies on physical-chemical properties and biological response of living tissues to NiTi (Nitinol) carried out recently, aiming at an understanding of the place of this material among the implant alloys in use. Advantages of shape memory and superelasticity are analyzed in respect to functionality of implants in the body. Various approaches to surface treatment, sterilization procedures, and resulting surface conditions are analyzed. A review of corrosion studies conducted both on wrought and as-cast alloys using potentiodynamic and potentiostatic techniques in various corrosive media and in actual body fluids is also given. The parameters of localized and galvanic corrosion are presented. The corrosion behavior is analyzed with respect to alloy composition, phase state, surface treatment, and strain and compared to that of conventional implant alloys. Biocompatibility of porous Nitinol, Ni release and its effect on living cells are analyzed based on understanding of the surface conditions and corrosion behavior. Additionally, the paper offers a brief overview of the comparative toxicity of metals, components of commonly used medical alloys, indicating that the biocompatibility profile of Nitinol is conducive to present in vivo applications. PMID:11847410

  18. Polyion Selective Polymeric Membrane-Based Pulstrode as a Detector in Flow-Injection Analysis

    PubMed Central

    2015-01-01

    A method for the detection of polyions using fully reversible polyion selective polymeric membrane type pulstrodes as detectors in a flow-injection analysis (FIA) system is examined. The detection electrode consists of a plasticized polymeric membrane doped with 10 wt % of tridodecylmethylammonium-dinonylnaphthalene sulfonate (TDMA/DNNS) ion-exchanger salt. The pulse sequence used involves a short (1 s) galvanostatic pulse, an open-circuit pulse (0.5 s) during which the EMF of the cell is measured, and a longer (15 s) potentiostatic pulse to return the membrane to its original chemical composition. It is shown that total pulse sequence times can be optimized to yield reproducible real-time detection of injected samples of protamine and heparin at up to 20 samples/h. Further, it is shown that the same membrane detector can be employed for FIA detection of both polycations at levels ≥10 μg/mL and polyanions at levels of ≥40 μg/mL by changing the direction of the galvanostatic pulse. The methodology described may also be applicable in the detection of polyionic species at low levels in other flowing configurations, such as in liquid chromatography and capillary electrophoresis. PMID:24650129

  19. Polymer film selection for corrosion protection of data storage magnetic materials.

    PubMed

    Chatruprachewin, Santi; Supadee, Laddawan; Titiroongruang, Wisut

    2011-12-01

    Due to the current requirement of high recording density of hard disk drive, the thickness of DLC layer which is the protective layer is needed to be reduced. Therefore, the corrosion of read-write elements that are fabricated from soft magnetic materials is more critical. During the photolithography process, polymer photoresist is playing the major role on controlling the corrosion of soft magnetic materials. Two different types of polymer photoresists are selected to investigate, noted as wet photoresist and dry photoresist, respectively. Contact angle measurement, AFM and SEM are techniques using to determine the quality of polymer photoresists. Furthermore, the direct corrosion is also studied by using potentiostat/galvanostat-based measurements. The result suggested that the wet photoresist, AZ4999 Clariant, is better as compared to that of dry photoresist. No surface degradation as well as surface defects of the wet photoresist was found after lithography process. The corrosion rate of the specimen coated by this corresponding wet film is found to be only 1.44 x 10(-6) mm/y. In addition, the wet photoresist surface is hydrophobic posed of more than 75 degree of contact angle. PMID:22408952

  20. Effect of Non-ionic Surfactants and Its Role in K Intercalation in Electrolytic Manganese Dioxide

    NASA Astrophysics Data System (ADS)

    Biswal, Avijit; Tripathy, B. C.; Subbaiah, T.; Meyrick, D.; Ionescu, Mihail; Minakshi, Manickam

    2014-09-01

    The effect of non-ionic surface active agents (surfactants) Triton X-100 (TX-100) and Tween-20 (Tw-20) and their role in potassium intercalation in electrolytic manganese dioxide (EMD) produced from manganese cake has been investigated. Electrosynthesis of MnO2 in the absence or presence of surfactant was carried out from acidic MnSO4 solution obtained from manganese cake under optimized conditions. A range of characterization techniques, including field emission scanning electron microscopy, transmission electron microscopy (TEM), Rutherford back scattering (RBS), and BET surface area/porosity studies, was carried out to determine the structural and chemical characteristics of the EMD. Galvanostatic (discharge) and potentiostatic (cyclic voltammetric) studies were employed to evaluate the suitability of EMD in combination with KOH electrolyte for alkaline battery applications. The presence of surfactant played an important role in modifying the physicochemical properties of the EMD by increasing the surface area of the material and hence, enhancing its electrochemical performance. The TEM and RBS analyses of the discharged EMD (γ-MnO2) material showed clear evidence of potassium intercalation or at least the formation of a film on the MnO2 surface. The extent of intercalation was greater for EMD deposited in the presence of TX-100. Discharged MnO2 showed products of Mn2+ intermediates such as MnOOH and Mn3O4.

  1. Comparison of Electrochemical Methods to Determine Crevice Corrosion Repassivation Potential of Alloy 22 in Chloride Solutions

    SciTech Connect

    K. Evans; A. Yilmaz; S. Day; L. Wong; J. Estill

    2004-08-23

    Alloy 22 (N06022) is a nickel-based alloy highly resistant to corrosion. In some aggressive conditions of high chloride concentration, temperature and applied potential, Alloy 22 may suffer crevice corrosion, a form of localized corrosion. There are several electrochemical methods that can be used to determine localized corrosion in metallic alloys. One of the most popular for rapid screening is the cyclic potentiodynamic polarization (CPP). This work compares the repassivation potentials obtained using CPP to related repassivation potential values obtained using the Tsujikawa-Hisamatsu Electrochemical (THE) method and the potentiostatic (POT) method. Studied variables included temperature and chloride concentration. The temperature was varied from 30 C and 120 C and the chloride concentration was varied between 0.0005 M to 4 M. Results show that similar repassivation potentials were obtained for Alloy 22 using CPP and THE methods. Generally, under more aggressive conditions, the repassivation potentials were more conservative using the CPP method. POT tests confirmed the validity of the repassivation potential as a threshold below which localized corrosion does not nucleate. The mode of attack in the tested specimens varied depending if the test method was CPP or THE; however, the repassivation potential remained the same.

  2. Tribocorrosion mechanisms of Ti6Al4V biomedical alloys in artificial saliva with different pHs

    NASA Astrophysics Data System (ADS)

    Licausi, M. P.; Igual Muñoz, A.; Amigó Borrás, V.

    2013-10-01

    Titanium and its alloys has been widely used for the design of dental implants because of its biocompatibility, mechanical properties and corrosion resistance. The powder-metallurgy process is a promising alternative to the casting fabrication process of titanium alloys for bone implants design as the porous structure mimics the natural bone structures, allowing the bone to grow into the pores which results in a better fixation of the artificial implant. However, under in vivo conditions the implants are subjected to tribocorrosion phenomenon, which consists in the degradation mechanisms due to the combined effect of wear and corrosion. The aim of this study is to evaluate the tribocorrosion behaviour of cast and sintered Ti6Al4V biomedical alloy for dental applications using the cast material as reference. Titanium samples were tested in artificial human saliva solution with three different pHs (3, 6, 9) and in an acidic saliva with 1000 ppm fluorides (AS-3-1000F-) by different electrochemical techniques (potentiodynamic curves, potentiostatic tests and tribo-electrochemical tests). Cast and sintered titanium alloys exhibit the same tribocorrosion mechanisms in AS independently of the pH which consists in plastic deformation with passive dissolution, but the addition of fluorides to the acidified solution changes the degradation mechanism towards active dissolution of the titanium alloys.

  3. Dithionite/air direct ion liquid fuel cell

    NASA Astrophysics Data System (ADS)

    Noack, Jens; Tübke, Jens; Pinkwart, Karsten

    2015-07-01

    The feasibility of an alkaline S2O42-/air-fuel cell was evaluated at room temperature, using a cell with an anion exchange membrane and a platinum oxygen reduction reaction catalyst. The tests performed were open circuit voltage analysis, linear sweep voltammetry, discharge analysis and electrochemical impedance spectroscopy (EIS) with registration of anode half-cell potential. With 0.85 M Na2S2O4 in 2 M KOH, the cell achieved a maximum power density of 2 mW cm-2, and the open circuit cell voltage was about 0.9 V. In a potentiostatic discharging at 0.2 V cell voltage, an energy efficiency of 12.3% was achieved at an energy density of 8.6 Wh L-1. The low power density was mainly due to the low reaction kinetics of dithionite oxidation at graphite electrodes. The low energy efficiency was mainly caused by a low cathode potential, which probably resulted from mixed potential formation and the low anode kinetics.

  4. Strong Photo-Amplification Effects in Flexible Organic Capacitors with Small Molecular Solid-State Electrolyte Layers Sandwiched between Photo-Sensitive Conjugated Polymer Nanolayers

    NASA Astrophysics Data System (ADS)

    Lee, Hyena; Kim, Jungnam; Kim, Hwajeong; Kim, Youngkyoo

    2016-02-01

    We demonstrate strong photo-amplification effects in flexible organic capacitors which consist of small molecular solid-state electrolyte layers sandwiched between light-sensitive conjugated polymer nanolayers. The small molecular electrolyte layers were prepared from aqueous solutions of tris(8-hydroxyquinoline-5-sulfonic acid) aluminum (ALQSA3), while poly(3-hexylthiophene) (P3HT) was employed as the light-sensitive polymer nanolayer that is spin-coated on the indium-tin oxide (ITO)-coated poly(ethylene terephthalate) (PET) film substrates. The resulting capacitors feature a multilayer device structure of PET/ITO/P3HT/ALQSA3/P3HT/ITO/PET, which were mechanically robust due to good adhesion between the ALQSA3 layers and the P3HT nanolayers. Results showed that the specific capacitance was increased by ca. 3-fold when a white light was illuminated to the flexible organic multilayer capacitors. In particular, the capacity of charge storage was remarkably (ca. 250-fold) enhanced by a white light illumination in the potentiostatic charge/discharge operation, and the photo-amplification functions were well maintained even after bending for 300 times at a bending angle of 180o.

  5. Electrosynthesis of polyaniline-mutilwalled carbon nanotube nanocomposite films in the presence of sodium dodecyl sulfate for glucose biosensing

    NASA Astrophysics Data System (ADS)

    Huyen Le, Trong; Thang Trinh, Ngoc; Nguyen, Le Huy; Binh Nguyen, Hai; Nguyen, Van Anh; Tran, Dai Lam; Dung Nguyen, Tuan

    2013-06-01

    Polyaniline-mutilwalled carbon nanotube (PANi-MWCNT) nanocomposites were electropolymerized in the presence of sodium dodecyl sulfate (SDS) onto interdigitated platinum-film planar microelectrodes (IDμE). The MWCNTs were first dispersed in SDS solution then mixed with aniline and H2SO4. This mixture was used to electro-synthesize PANi-MWCNT films with potentiostatic method at E = + 0.90 V (versus SCE). The PANi-MWCNT films were characterized by cyclic voltammetry (CV) and scanning electron microscopy (SEM). The results show that the PANi-MWCNT films have a high electroactivity, and a porous and branched structure that can increase the specific surface area for biosensing application. In this work the PANi-MWCNT films were applied for covalent immobilization of glucose oxidase (GOx) via glutaraldehyde agent. The GOx/PANi-MWCNT/IDμE was studied using cyclic voltammetric and chronoamperometric techniques. The effect of several interferences, such as ascorbic acid (AA), uric acid (UA), and acetaminophen (AAP) on the glucosensing at +0.6 V (versus SCE) is not significant. The time required to reach 95% of the maximum steady-state current was less than 5 s. A linear range of the calibration curve for the glucose concentration lies between 1 and 12 mM which is a suitable level in the human body.

  6. Enhanced low-temperature power density of solid oxide fuel cell by nickel nanoparticle infiltration into pre-fired Ni/yttria-stabilized zirconia anode.

    PubMed

    Kang, Lee-Seung; Park, Jae Layng; Lee, Sungkyu; Jin, Yun-Ho; Hong, Hyun-Seon; Lee, Chan-Gi; Kim, Bum Sung

    2014-12-01

    The Ni/yttria-stabilized zirconia (YSZ) anode morphology of an anode-supported solid oxide fuel cell (SOFC) unit cell was improved by nickel nanoparticle infiltration. A colloidal route was selected for efficient fabrication of nickel metal nanoparticles and subsequent infiltration into the Ni/YSZ anode of a pre-fired SOFC unit cell. The power density of the anode-supported SOFC unit cell was measured by the potentiostatic method to investigate the effect of nickel nanoparticle infiltration. The increase in the power density of the Ni/YSZ anode with nickel nanoparticle infiltration became gradually less significant as the SOFC operating temperature increased from 700 to 800 degrees C. The improved performance of the Ni/YSZ anode with nickel nanoparticle infiltration compared to that of an anode without nickel nanoparticles is tentatively attributed to two factors: The discretely distributed nanoparticles on the nanostructured electrodes exhibited significant catalytic effects on the electrochemical performance of the electrodes, in addition to substantially increasing the triple phase boundary lengths. PMID:25970993

  7. Wearable salivary uric acid mouthguard biosensor with integrated wireless electronics

    PubMed Central

    Kim, Jayoung; Imani, Somayeh; de Araujo, William R.; Warchall, Julian; Valdés-Ramírez, Gabriela; Paixão, Thiago R.L.C.; Mercier, Patrick P.; Wang, Joseph

    2016-01-01

    This article demonstrates an instrumented mouthguard capable of non-invasively monitoring salivary uric acid (SUA) levels. The enzyme (uricase)-modified screen printed electrode system has been integrated onto a mouthguard platform along with anatomically-miniaturized instrumentation electronics featuring a potentiostat, microcontroller, and a Bluetooth Low Energy (BLE) transceiver. Unlike RFID-based biosensing systems, which require large proximal power sources, the developed platform enables real-time wireless transmission of the sensed information to standard smartphones, laptops, and other consumer electronics for on-demand processing, diagnostics, or storage. The mouthguard biosensor system offers high sensitivity, selectivity, and stability towards uric acid detection in human saliva, covering the concentration ranges for both healthy people and hyperuricemia patients. The new wireless mouthguard biosensor system is able to monitor SUA level in real-time and continuous fashion, and can be readily expanded to an array of sensors for different analytes to enable an attractive wearable monitoring system for diverse health and fitness applications. PMID:26276541

  8. Electrochemical noise measurement: The definitive in-situ technique for corrosion applications?

    SciTech Connect

    Dawson, J.L.

    1996-12-31

    A review is presented of electrochemical noise (EN), the generic term given to fluctuations of current and potential seen in high-temperature corrosion, molten salt corrosion, and aqueous corrosion. EN levels in corrosion and particularly localized corrosion are significantly greater than EN observed in redox systems. EN associated with corrosion is the result of stochastic pulses of current generated by, for example, sudden film rupture, crack propagation, discrete events involving metal dissolution at etch pits, grain boundaries and kink sites, and hydrogen discharge with gas bubble formation and detachment. EN in corrosion includes low-frequency, nonstationary, and weakly stationary processes; transients; and cyclic or oscillatory phenomena. The use of EN, obtained either by potentiostatic/galvanostatic measurements or at freely corroding potentials, has been shown to offer advantages over conventional DC and AC techniques in research studies, testing, and corrosion monitoring. In many cases, reaction mechanisms can be elucidated and corrosion rate information can be obtained. Assessment of individual transients, use of signal analysis techniques, modeling of ensembles of transients as developed for electrocrystallization studies, and use of the chaos theory have all been used in EN evaluations.

  9. Effect of metallurgical factors on the electrochemical noise measured on AISI Type 430 stainless steels in chloride-containing media

    SciTech Connect

    Gorse, D.; Boulleret, C.; Baroux, B.

    1996-12-31

    Potentiostatic noise measurements are performed on a series of AISI 430 type ferritic stainless steels containing controlled amounts of sulfur (from 8 up to 47 ppm) and titanium (up to 0.37 wt%), in 0.02M sodium chloride (NaCl) aqueous solution (pH 6.6), in a range of potentials below the pitting potential. The authors focus on the evolution of the shape of the current transients, going from a titanium (Ti) free and 41-ppm sulfur-containing alloy to different Ti-bearing alloys with comparable amount of sulfur ({approximately}40 ppm). The results are compared to the case of a Ti-free and low sulfur (8-ppm) containing alloy. The shape of the anodic current transients obeys a power law, t{sup n}. The authors distinguish two different situations, with n either less or larger than 1, which can be associated with the Ti and sulfur content in the steel. The influence of the exposure time under polarization is also discussed. It appears that for the manganese sulfide (MnS)-containing alloys, after prolonged polarization, the shape of the metastable pitting events evolves toward that found for MnS-free alloys (Ti-bearing), or low-sulfur-containing alloys. Attention is drawn to the possible relationship between the shape of the current transients and the metallurgical defects acting as pitting initiation sites.

  10. Photoelectrocatalytic oxidation of glucose at a ruthenium complex modified titanium dioxide electrode promoted by uric acid and ascorbic acid for photoelectrochemical fuel cells

    NASA Astrophysics Data System (ADS)

    Lu, Shuo-Jian; Ji, Shi-Bo; Liu, Jun-Chen; Li, Hong; Li, Wei-Shan

    2015-01-01

    The simultaneous presence of uric acid (UA) and ascorbic acid (AA) is first found to largely promote the photoelectrocatalytic oxidation of glucose (GLU) at an indium-tin oxide (ITO) or TiO2 nanoparticles/ITO electrode modified with [Ru(tatp)3]2+ (tatp = 1,4,8,9-tetra-aza-triphenylene) possessing good redox activity and nanoparticle size distribution. A well-defined electrocatalytic peak for GLU oxidation is shown at 0.265 V (vs. SCE) under approximate physiological conditions upon incorporation of UA and AA. The [Ru(tatp)3]2+/ITO electrode exhibits attractive amperometric oxidation responses towards GLU, UA and AA, while controlled potentiostatically at 0.3 V, 0.7 V and 1.0 V, respectively, indicating high sensitivity and excellent reproducibility. On basis of the photoelectrocatalysis of [Ru(tatp)3]2+/TiO2/ITO anode, a GLU concentration-dependent photoelectrochemical fuel cell vs. SCE is elaborately assembled. The proposed free-enzyme photoelectrochemical fuel cell employing 0.1 M GLU associated with 0.01 M UA and 0.01 M AA as fuel shows open-circuit photovoltage of 0.608 V, short-circuit photocurrent density of 124.5 μA cm-2 and maximum power density of 21.75 μW cm-2 at 0.455 V, fill factor of 0.32 and photoenergy conversion efficiency of 36.65%, respectively.

  11. Halogen-free boron based electrolyte solution for rechargeable magnesium batteries

    NASA Astrophysics Data System (ADS)

    Zhu, Jinjie; Guo, Yongsheng; Yang, Jun; Nuli, Yanna; Zhang, Fan; Wang, Jiulin; Hirano, Shin-ichi

    2014-02-01

    All halogen containing electrolytes for Mg battery are apt to corrode conventional metal current collectors. In this paper, a new type of halogen-free boron based electrolyte (Mg[Mes3BPh]2/THF) is designed and prepared. Electrochemical tests show that this electrolyte system possesses high ion conductivity (1.5 × 10-3 S cm-1) and good Mg deposition-dissolution reversibility. More importantly, the same electrochemical window (2.6 V vs. Mg RE) of the electrolyte on Pt and stainless steel electrodes indicates that halogen-free electrolyte indeed lessens the corrosion to conventional metal current collectors. The surface morphologies of stainless steel, aluminum and copper are further observed after their anodic potentiostatic polarization in 0.25 mol L-1 Mg[Mes3BPh]2/THF electrolyte solution for 2 days. A comparison with halogen containing electrolytes proves that the presence of halogen in electrolyte is the reason for corrosion. This work provides a stepping stone for developing new halogen-free electrolyte systems for rechargeable Mg batteries.

  12. The Prediction of Long-Term Coating Performance from Short-Term Electrochemical Data. Part 2; Comparison of Electrochemical Data to Field Exposure Results for Coatings on Steel

    NASA Technical Reports Server (NTRS)

    Contu, F.; Taylor, S. R.; Calle, L. M.; Hintze, P. E.; Curran, J. P.; Li, W.

    2009-01-01

    The pace of coatings development is limited by the time required to assess their corrosion protection properties. This study takes a step f orward from Part I in that it correlates the corrosion performance of organic coatings assessed by a series of short-term electrochemical measurement with 18-month beachside exposure results of duplicate pan els. A series of 19 coating systems on A36 steel substrates were test ed in a completely blind study using the damage tolerance test (DTT). In the DTT, a through-film pinhole defect is created, and the electro chemical characteristics of the defect are then monitored over the ne xt 4 to 7 days while immersed in 0.SM NaCl. The open circuit potentia l, anodic potentiostatic polarization tests and electrochemical imped ance spectroscopy were used to study the corrosion behavior of the co ating systems. The beachside exposure tests were conducted at the Ken nedy Space Center according to ASTM D610-01. It was found that for 79 % of the coatings systems examined, the 18 month beachside exposure r esults could be predicted by two independent laboratory tests obtained within 7 days.

  13. Repassivation behavior of 316L stainless steel in borate buffer solution: Kinetics analysis of anodic dissolution and film formation

    NASA Astrophysics Data System (ADS)

    Xu, Haisong; Sun, Dongbai; Yu, Hongying

    2015-12-01

    The repassivation behavior of metals or alloys after oxide film damage determines the development of local corrosion and corrosion resistance. In this work, the repassivation kinetics of 316L stainless steel (316L SS) are investigated in borate buffer solution (pH 9.1) by using the abrading electrode technique. The current densities flowing from bare 316L SS surface are measured by potentiostatic method and analyzed to characterize repassivation kinetics. The initial stages of current decay (t < 500 ms) are discussed according to a film growth model, which describes the initial current transient should be divided into substrate dissolution current and passive film formation current based on Avrami kinetics. Then the two independent components are analyzed individually. The film formation rate and the thickness of film are compared in different applied potential. It is shown that anodic dissolution dominates the repassivation for a short time during the early times, and a higher applied potential will promote the anodic dissolution of metal. The film growth rate increases slightly with increasing in potential. Correspondingly, increase in applied potential from 0 VSCE to 0.8 VSCE results in thicker monolayer, which covers the whole bare surface at the time of θ = 1. The electric field strengths through the thin passive film could reach 3.97 × 106 V cm-1.

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

    NASA Astrophysics Data System (ADS)

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

    2016-02-01

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

  15. Pt-Sn/C catalysts prepared by sodium borohydride reduction for alcohol oxidation in fuel cells: Effect of the precursor addition order

    NASA Astrophysics Data System (ADS)

    López-Suárez, F. E.; Bueno-López, A.; Eguiluz, K. I. B.; Salazar-Banda, G. R.

    2014-12-01

    A series of Pt-Sn/C catalysts used as anodes during ethanol oxidation are synthesized by a deposition process using NaBH4 as the reducing agent. The order in which the precursors are added affects the electrocatalytic activity and physical-chemical characteristics of the bimetallic catalysts, where the Pt-Sn catalyst prepared by co-precipitation of both metals functions best below a potential of 0.5 V and the catalyst prepared by sequential deposition of Sn and Pt (drying after Sn addition) is most active above a potential of 0.5 V. The electrochemical behavior of catalysts during ethanol oxidation in an acidic medium are characterized and monitored in a half-cell test at room temperature by cyclic voltammetry, chronoamperometry and anode potentiostatic polarization. Catalyst structure and chemical composition are investigated by transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). This behavior presented for best Pt-Sn catalyst can be attributed to the so-called bifunctional mechanism and to the electronic interaction between Pt and Sn.

  16. Experimental investigation of the effect of indium content on the CuIn{sub 5}S{sub 8} electrodes using electrochemical impedance spectroscopy

    SciTech Connect

    Gannouni, M. Assaker, I. Ben; Chtourou, R.

    2015-01-15

    This paper reports on the use of electrochemical impedance spectroscopy to investigate the electrochemical behavior of spinel CuIn{sub 5}S{sub 8}/electrolyte interface. The CuIn{sub 5}S{sub 8} spinel films have been potentiostatically deposited onto indium tin oxide (ITO)-coated glass substrate. CuCl{sub 2} and InCl{sub 3} mixed solutions with different [Cu]/[In] ratios were used as cation precursor and Na{sub 2}S{sub 2}O{sub 3} as the anion precursor in acidic solution and at room temperature. The effect of the [Cu]/[In] ratio in the precursor solution on the structural, chemical stoichiometry, and morphological properties of prepared samples, as well as the electrochemical behavior of the CuIn{sub 5}S{sub 8}/electrolyte interface was investigated. The electrochemical impedance spectroscopy data have been modeled using an equivalent circuit approach. Several parameters such as, flat-band potential and free carrier concentration were determined by the change in the Mott–Schottky plots.

  17. Stress-corrosion behavior of aluminum-lithium alloys in aqueous environments

    NASA Technical Reports Server (NTRS)

    Pizzo, P. P.; Galvin, R. P.; Nelson, H. G.

    1983-01-01

    The stress corrosion susceptibility of two powder metallurgy (P/M) alloys, Al-Li-Cu and Al-Li-Cu-Mg two mechanically attrited (M/A) alloys, Al-Li-Cu and Al-Li-Mg; and two wrought, ingot alloys, X-2020 and AA7475, are compared. Time-dependent fracture in an aqueous sodium chloride environment under alternate immersion condition was found to vary significantly between alloys. The stress corrosion behavior of the two powder metallurgy processed alloys was studied in detail under conditions of crack initiation, static crack growth, and fatigue crack growth. A variety of stress corrosion tests were performed including smooth surface, time-to-failure tests; potentiostatic tests on smooth surfaces exposed to constant applied strain rates; and fracture mechanics-type tests under static and cyclic loads. Both alloys show surface pitting and subsequent intergranular corrosion. Pitting is more severe in the magnesium-bearing alloy and is associated with stringer particles strung along the extrusion direction as a result of P/M processing.

  18. Fabrication of Cu2O/γ-FeOOH heterojunction solar cells using electrodeposition

    NASA Astrophysics Data System (ADS)

    Vequizo, Junie Jhon M.; Ichimura, Masaya

    2014-04-01

    Cu2O/γ-FeOOH heterojunction solar cells were fabricated using galvanostatic-potentiostatic electrodeposition methods. The γ-FeOOH films showed n-type conductivity with a band gap of 2.2 eV. The electrodeposited Cu2O/γ-FeOOH heterojunction exhibited photovoltaic characteristics with a short-circuit current density of 0.95 mA/cm2 and open-circuit voltage of 0.11 V. Using core-level spectroscopy, it was demonstrated that the Cu2O/FeOOH heterostructure exhibited a type II junction with a valence band offset of 0.8 eV. The conduction band minimum of Cu2O was predicted to be higher than that of γ-FeOOH by 0.7 eV. This finding indicates that the γ-FeOOH material can be regarded as a suitable hetero-partner of other p-type absorbers.

  19. Effects of Osseointegration by Bone Morphogenetic Protein-2 on Titanium Implants In Vitro and In Vivo

    PubMed Central

    Teng, Fu-Yuan; Chen, Wen-Cheng; Wang, Yin-Lai; Hung, Chun-Cheng; Tseng, Chun-Chieh

    2016-01-01

    This study designed a biomimetic implant for reducing healing time and achieving early osseointegration to create an active surface. Bone morphogenetic protein-2 (BMP-2) is a strong regulator protein in osteogenic pathways. Due to hardly maintaining BMP-2 biological function and specificity, BMP-2 efficient delivery on implant surfaces is the main challenge for the clinic application. In this study, a novel method for synthesizing functionalized silane film for superior modification with BMP-2 on titanium surfaces is proposed. Three groups were compared with and without BMP-2 on modified titanium surfaces in vitro and in vivo: mechanical grinding; electrochemical modification through potentiostatic anodization (ECH); and sandblasting, alkali heating, and etching (SMART). Cell tests indicated that the ECH and SMART groups with BMP-2 markedly promoted D1 cell activity and differentiation compared with the groups without BMP-2. Moreover, the SMART group with a BMP-2 surface markedly promoted early alkaline phosphatase expression in the D1 cells compared with the other surface groups. Compared with these groups in vivo, SMART silaning with BMP-2 showed superior bone quality and created contact areas between implant and surrounding bones. The SMART group with BMP-2 could promote cell mineralization in vitro and osseointegration in vivo, indicating potential clinical use. PMID:26977141

  20. Synthesis of one-dimensional gold nanostructures and the electrochemical application of the nanohybrid containing functionalized graphene oxide for cholesterol biosensing.

    PubMed

    Nandini, Seetharamaiah; Nalini, Seetharamaiah; Reddy, M B Madhusudana; Suresh, Gurukar Shivappa; Melo, Jose Savio; Niranjana, Pathappa; Sanetuntikul, Jakkid; Shanmugam, Sangaraju

    2016-08-01

    This manuscript reports a new approach for the synthesis of one dimensional gold nanostructure (AuNs) and its application in the development of cholesterol biosensor. Au nanostructures have been synthesized by exploiting β-diphenylalanine (β-FF) as an sacrificial template, whereas the Au nanoparticles (AuNPs) were synthesized by ultrasound irradiation. X-ray diffractometer (XRD), scanning electron microscope (SEM) and energy dispersive analysis of X-rays (EDAX) have been employed to characterize the morphology and composition of the prepared samples. With the aim to develop a highly sensitive cholesterol biosensor, cholesterol oxidase (ChOx) was immobilized on AuNs which were appended on the graphite (Gr) electrode via chemisorption onto thiol-functionalized graphene oxide (GO-SH). This Gr/GO-SH/AuNs/ChOx biosensor has been characterized using cyclic voltammetry (CV), electrochemical impedance spectroscopy and chronoamperometry. CV results indicated a direct electron transfer between the enzyme and the electrode surface. A new potentiostat intermitant titration technique (PITT) has been studied to determine the diffusion coefficient and maxima potential value. The proposed biosensor showed rapid response, high sensitivity, wide linear range and low detection limit. Furthermore, our AuNs modified electrode showed excellent selectivity, repeatability, reproducibility and long term stability. The proposed electrode has also been used successfully to determine cholesterol in serum samples. PMID:27100467

  1. Effects of concentration-dependent elastic modulus on Li-ions diffusion and diffusion-induced stresses in spherical composition-gradient electrodes

    SciTech Connect

    Zhang, Kai; Li, Yong; Zheng, Bailin

    2015-09-14

    The composition-gradient electrode material is considered as one of the most promising materials for lithium-ion batteries because of its excellent electrochemical performance and thermal stability. In this work, the effects of concentration-dependent elastic modulus on Li-ions diffusion and diffusion-induce stress in the composition-gradient electrodes were studied. The coupling equations of elasticity and diffusion under both potentiostatic charging and galvanostatic charging were developed to obtain the distributions of both the Li-ions concentration and the stress. The results indicated that the effects of the concentration-dependent elastic modulus on the Li-ions diffusion and the diffusion-induce stresses are controlled by the lithiation induced stiffening factor in the composition-gradient electrodes: a low stiffening factor at the center and a high stiffening factor at the surface lead to a significant effect, whereas a high stiffening factor at the center and a low stiffening factor at the surface result in a minimal effect. The results in this work provide guidance for the selection of electrode materials.

  2. Solid-state electrochemical kinetics of Li-ion intercalation into Li{sub 1{minus}x}CoO{sub 2}: Simultaneous application of electroanalytical techniques SSCV, PITT, and EIS

    SciTech Connect

    Levi, M.D.; Salitra, G.; Markovsky, B.; Teller, H.; Aurbach, D.; Heider, U.; Heider, L.

    1999-04-01

    The electroanalytical behavior of thin Li{sub 1{minus}x}CoO{sub 2} electrodes is elucidated by the simultaneous application of three electroanalytical techniques: slow-scan-rate cyclic voltammetry (SSCV), potentiostatic intermittent titration technique, and electrochemical impedance spectroscopy. The data were treated within the framework of a simple model expressed by a Frumkin-type sorption isotherm. The experimental SSCV curves were well described by an equation combining such an isotherm with the Butler-Volmer equation for slow interfacial Li-ion transfer. The apparent attraction constant was {minus}4.2, which is characteristic of a quasi-equilibrium, first-order phase transition. Impedance spectra reflected a process with the following steps: Li{sup +} ion migration in solution, Li{sup +} ion migration through surface films, strongly potential-dependent charge-transfer resistance, solid-state Li{sup +} diffusion, and accumulation of the intercalants into the host materials. An excellent fit was found between these spectra and an equivalent circuit, including a Voigt-type analog (Li{sup +} migration through multilayer surface films and charge transfer) in series with a finite-length Warburg-type element (Li{sup +} solid-state diffusion), and a capacitor (Li accumulation). In this paper, the authors compare the solid-state diffusion time constants and the differential intercalation capacities obtained by the three electroanalytical techniques.

  3. Lab-on-a-Bird: Biophysical Monitoring of Flying Birds

    PubMed Central

    Gumus, Abdurrahman; Lee, Seoho; Ahsan, Syed S.; Karlsson, Kolbeinn; Gabrielson, Richard; Guglielmo, Christopher G.; Winkler, David W.; Erickson, David

    2015-01-01

    The metabolism of birds is finely tuned to their activities and environments, and thus research on avian systems can play an important role in understanding organismal responses to environmental changes. At present, however, the physiological monitoring of bird metabolism is limited by the inability to take real-time measurements of key metabolites during flight. In this study, we present an implantable biosensor system that can be used for continuous monitoring of uric acid levels of birds during various activities including flight. The system consists of a needle-type enzymatic biosensor for the amperometric detection of uric acid in interstitial fluids. A lightweight two-electrode potentiostat system drives the biosensor, reads the corresponding output current and wirelessly transfers the data or records to flash memory. We show how the device can be used to monitor, in real time, the effects of short-term flight and rest cycles on the uric acid levels of pigeons. In addition, we demonstrate that our device has the ability to measure uric acid level increase in homing pigeons while they fly freely. Successful application of the sensor in migratory birds could open up a new way of studying birds in flight which would lead to a better understanding of the ecology and biology of avian movements. PMID:25880904

  4. Corrosion and Erosion-Corrosion Processes of Metal-Matrix Composites in Slurry Conditions

    NASA Astrophysics Data System (ADS)

    Flores, J. F.; Neville, A.; Kapur, N.; Gnanavelu, A.

    2012-03-01

    The corrosion and erosion-corrosion (EC) processes of four metal-matrix composites (MMCs) in a simulated cooling water environment have been assessed in this article. The MMCs consisted of two Ni-base and two Fe-base matrices alloyed with different concentrations of chromium, molybdenum, boron, silicon, and carbon; the matrices were reinforced with tungsten carbide (WC) particles. The corrosion behavior has been investigated using a combination of potentiostatic polarization and post-tests surface analysis. The EC processes were studied by in situ electrochemical techniques measuring the current density and corrosion potential response at different slurry temperatures and sand content. At static conditions it was found that as the temperature increased, there was a transition from a homogeneous corrosion of the matrix to an interfacial corrosion mechanism. The Ni-base MMCs showed a better corrosion resistance and interestingly a highly alloyed matrix did not significantly improved MMC's corrosion resistance. In the in situ EC tests, the Fe-base MMCs showed a constant increase in the current density at all sand contents. Whereas, significant changes were not observed in the Ni-base MMCs below 0.5 g/L. Although sand content had an effect on the monitored current density (the current increased as the sand content increased) this effect was less pronounced above 3 g/L.

  5. Fabrication of CIGS Films by Electrodeposition Method for Photovoltaic Cells

    NASA Astrophysics Data System (ADS)

    Lee, Hyunju; Yoon, Hyukjoo; Ji, Changwook; Lee, Dongyun; Lee, Jae-Ho; Yun, Jae-Ho; Kim, Yangdo

    2012-12-01

    Cu(InGa)Se2 (CIGS) thin films were fabricated by electrochemical deposition in a single bath containing Cu, In, Ga, and Se ions. The electrolyte was prepared by dissolving CuCl2, InCl3, GaCl3, H2SeO3, and LiCl in deionized water. The potentiostatic deposition process was achieved by applying a voltage ranging from -0.5 V to -0.8 V versus Ag/AgCl. The effects of different chemical bath concentrations on the film composition and morphology were investigated. Stoichiometric CIGS film composition could be achieved by controlling the chemical compositions of the bath and the voltage. Gelatin was added to the solution to improve the surface and microstructures of the CIGS film. The as-deposited films were annealed at 500°C in Ar atmosphere for crystallization. The structural, morphological, and compositional properties of the CIGS thin films before and after annealing were examined by x-ray diffraction, scanning electron microscopy, and energy-dispersive spectroscopy. This study showed that the composition of the CIGS films is dependent on the bath concentration, whereas the applied potential had relatively less effect on the CIGS film composition. In addition, the use of gelatin helped in the fabrication of crack-free CIGS thin films with greatly improved surface morphology.

  6. Effect of hydroxyapatite thickness on metal ion release from Ti6Al4V substrates.

    PubMed

    Sousa, S R; Barbosa, M A

    1996-02-01

    The electrochemical dissolution behaviour of Ti6Al4V alloy coated with hydroxyapatite (HA) by plasma spraying was studied in Hank's balanced salt solution (HBSS) and compared with that of polished and grit-blasted passivated surfaces. Two different nominal thicknesses of HA (50 and 200 micro m) were used. Taking a polished passivated surface as reference, grit blasting of the substrate increased the electrical charge used in the oxidation of Ti6Al4V alloy at constant potential, as a result of increased surface area. However, only HA coatings with a thickness of 200 micro m were capable of reducing the charge to values lower than those measured for polished surfaces. Electrochemical impedance spectroscopy has also shown that only 200 micro m thick coatings are effective in reducing the oxidation rate of the substrate. Furthermore, in potentiostatic experiments the 50 micro m thick coating detached from the substrate, which did not occur with the 200 micro m thick coating. However, after 6 months immersion in HBSS, detachment occurred in some regions of both coatings. No titanium, aluminium or vanadium were detected in solution by electrothermal atomic absorption spectroscopy. These data indicate that HA is an effective barrier to metal ion release, even for the thinner coatings, due to formation of metal phosphates or to incorporation of metal ions in the HA structure. PMID:8938233

  7. Ultrathin, Stretchable, Multiplexing pH Sensor Arrays on Biomedical Devices With Demonstrations on Rabbit and Human Hearts Undergoing Ischemia

    PubMed Central

    Chung, Hyun-Joong; Sulkin, Matthew S.; Kim, Jong-Seon; Goudeseune, Camille; Chao, Hsin-Yun; Song, Joseph W.; Yang, Sang Yoon; Hsu, Yung-Yu; Ghaffari, Roozbeh

    2014-01-01

    Stable pH is an established biomarker of health, relevant to all tissues of the body, including the heart. Clinical monitoring of pH in a practical manner, with high spatiotemporal resolution, is particularly difficult in organs such as the heart due to its soft mechanics, curvilinear geometry, heterogeneous surfaces and continuous, complex rhythmic motion. The results presented here illustrate that advanced strategies in materials assembly and electrochemical growth can yield interconnected arrays of miniaturized IrOx pH sensors encapsulated in thin, low-modulus elastomers to yield conformal monitoring systems capable of non-invasive measurements on the surface of the beating heart. A thirty channel custom data acquisition system enables spatiotemporal pH mapping with a single potentiostat. In-vitro testing reveals super-Nernstian sensitivity with excellent uniformity (69.9 ± 2.2 mV/pH), linear response to temperature (−1.6 mV/°C), and minimal influence of extracellular ions (< 3.5 mV). Device examples include sensor arrays on balloon catheters and on skin-like stretchable membranes. Real-time measurement of pH on the surfaces of explanted rabbit hearts and a donated human heart during protocols of ischemia-reperfusion illustrate some of the capabilities. Envisioned applications range from devices for biological research, to surgical tools and long-term implants. PMID:23868871

  8. The role of alloyed molybdenum in the dissolution and the passivation of nickel-molybdenum alloys in the presence of adsorbed sulfur

    SciTech Connect

    Marcus, P.; Moscatelli, M. )

    1989-06-01

    The authors discuss the effects of Mo on the dissolution and the passivation of a Ni-2 atom percent (a/o) Mo(100) alloy in 0.05M H/sub 2/SO/sub 4/ investigated with or without adsorbed sulfur. Sulfur was preadsorbed on the alloy surface in H/sub 2/S-H/sub 2/ gas mixtures. Complete monolayers of S (i.e., 43 X 10/sup -9/ g/cm/sup 2/) were formed with pH/sub 2/ = 2 X 10/sup -4/ and T = 600{sup 0}C. The surface coverages by sulfur were measured using the sulfur 35 radioisotope (/sup 35/S) and the chemical state was analyzed by electron spectroscopy for chemical analysis. Potentiodynamic and potentiostatic measurements were performed, and the concentration of sulfur on the surface was measured as a function of the amount of dissolving molybdenum. The effect of S is found to be very weak compared to the one previously observed on Ni and Ni-Fe alloys, which shows that molybdenum counteracts the detrimental effects of adsorbed sulfur.

  9. Preparation of Supercapacitors on Flexible Substrates with Electrodeposited PEDOT/Graphene Composites.

    PubMed

    Lehtimäki, Suvi; Suominen, Milla; Damlin, Pia; Tuukkanen, Sampo; Kvarnström, Carita; Lupo, Donald

    2015-10-14

    Composite films consisting of poly(3,4-ethylenedioxythiophene) (PEDOT) and graphene oxide (GO) were electrochemically polymerized by electrooxidation of EDOT in ionic liquid (BMIMBF4) onto flexible electrode substrates. Two polymerization approaches were compared, and the cyclic voltammetry (CV) method was found to be superior to potentiostatic polymerization for the growth of PEDOT/GO films. After deposition, incorporated GO was reduced to rGO by a rapid electrochemical method of repetitive cathodic potential cycling, without using any reducing reagents. The films were characterized in 3-electrode configuration in BMIMBF4. Symmetric supercapacitors with aqueous electrolyte were assembled from the composite films and characterized through cyclic voltammetry and galvanostatic discharge tests. It was shown that PEDOT/rGO composites have better capacitive properties than pure PEDOT or the unreduced composite film. The cycling stability of the supercapacitors was also tested, and the results indicate that the specific capacitance still retains well over 90% of the initial value after 2000 consecutive charging/discharging cycles. The supercapacitors were demonstrated as energy storages in a room light energy harvester with a printed organic solar cell and printed electrochromic display. The results are promising for the development of energy-autonomous, low-power, and disposable electronics. PMID:26381462

  10. Electrochemical nucleophilic synthesis of di-tert-butyl-(4-[18F]fluoro-1,2-phenylene)-dicarbonate

    PubMed Central

    He, Qinggang; Wang, Ying; Alfeazi, Ines; Sadeghi, Saman

    2015-01-01

    An electrochemical method with the ability to conduct 18F-fluorination of aromatic molecules through direct nucleophilic fluorination of cationic intermediates is presented in this paper. The reaction was performed on a remote-controlled automatic platform. Nucleophilic electrochemical fluorination of tert-butyloxycarbonyl (Boc) protected catechol, an intermediate model molecule for the positron emission tomography (PET) probe (3,4-dihydroxy-6-[18F]fluoro-l-phenylalanine), was performed. Fluorination was achieved under potentiostatic anodic oxidation in acetonitrile containing Et3N · 3HF and other supporting electrolytes. Radiofluorination efficiency was influenced by a number of variables, including the concentration of the precursor, concentration of Et3N · 3HF, type of supporting electrolyte, temperature and time, as well as applied potentials. Radiofluorination efficiency of 10.4 ± 0.6% (n = 4) and specific activity of up to 43 GBq/mmol was obtained after 1 h electrolysis of 0.1 M of 4-tert-butyl-diboc-catechol in the acetonitrile solution of Et3N · 3HF (0.033 M) and NBu4PF6 (0.05 M). Density functional theory (DFT) was employed to explain the tert-butyl functional group facilitation of electrochemical oxidation and subsequent fluorination. PMID:25000498

  11. Eliminating Electrochromic Degradation in Amorphous TiO2 through Li-Ion Detrapping.

    PubMed

    Wen, Rui-Tao; Niklasson, Gunnar A; Granqvist, Claes G

    2016-03-01

    The quest for superior and low-cost electrochromic (EC) thin films, for applications in smart windows, remains strong because of their large importance for energy-efficient buildings. Although the development of new EC materials for improved devices is important, diminishing or reversing degradation is another key issue, and electrical rejuvenation of degraded EC materials can offer new opportunities. Here we demonstrate that cathodically coloring EC thin films of TiO2, which normally suffer from ion-trapping-induced degradation of charge capacity and optical modulation upon extensive electrochemical cycling, can recover their initial EC performance by a rejuvenation procedure involving Li(+) ion detrapping. Thus, the initial performance can be regained, and refreshed TiO2 films exhibit the same degradation features as as-deposited films upon prolonged electrochemical cycling. The rejuvenation was carried out by using either galvanostatic or potentiostatic treatments. Our study may open avenues to explore the recovery not only of EC materials and devices based on those but also for other ion-exchange-based devices. PMID:26910644

  12. Corrosion of Carbon Steel and Corrosion-Resistant Rebars in Concrete Structures Under Chloride Ion Attack

    NASA Astrophysics Data System (ADS)

    Mohamed, Nedal; Boulfiza, Mohamed; Evitts, Richard

    2013-03-01

    Corrosion of reinforced concrete is the most challenging durability problem that threatens reinforced concrete structures, especially structures that are subject to severe environmental conditions (i.e., highway bridges, marine structures, etc.). Corrosion of reinforcing steel leads to cracking and spalling of the concrete cover and billions of dollars are spent every year on repairing such damaged structures. New types of reinforcements have been developed to avoid these high-cost repairs. Thus, it is important to study the corrosion behavior of these new types of reinforcements and compare them to the traditional carbon steel reinforcements. This study aimed at characterizing the corrosion behavior of three competing reinforcing steels; conventional carbon steel, micro-composite steel (MMFX-2) and 316LN stainless steel, through experiments in carbonated and non-carbonated concrete exposed to chloride-laden environments. Synthetic pore water solutions have been used to simulate both cases of sound and carbonated concrete under chloride ions attack. A three-electrode corrosion cell is used for determining the corrosion characteristics and rates. Multiple electrochemical techniques were applied using a Gamry PC4™ potentiostat manufactured by Gamry Instruments (Warminster, PA). DC corrosion measurements were applied on samples subjected to fixed chloride concentration in the solution.

  13. Electrodeposition and characterization of HgSe thin films

    SciTech Connect

    Mahalingam, T. . E-mail: maha51@rediffmail.com; Kathalingam, A.; Sanjeeviraja, C.; Chandramohan, R.; Chu, J.P.; Kim, Yong Deak; Velumani, S.

    2007-08-15

    In this article we present the results on the electrochemical synthesis of mercury selenide (HgSe), an interesting II-VI material. HgSe thin films were deposited potentiostatically on conducting glass substrates from an aqueous bath containing HgCl{sub 2} and SeO{sub 2}. The prepared films were characterized by X-ray diffraction (XRD), energy dispersive X-ray analysis (EDX), scanning electron microscope (SEM) and optical absorption techniques. Stoichiometric polycrystalline HgSe films were obtained at a deposition potential around - 0.7 V vs SCE, at a temperature 60 deg. C and a pH value of 3.5. The as-grown films exhibited a direct optical band gap of 0.78 eV. This report deals with the growth mechanism and a study related to the influence of electrolyte bath composition, deposition potential, temperature and pH on the properties of HgSe thin films.

  14. Carbon nanotube-based supercapacitors using low cost collectors

    NASA Astrophysics Data System (ADS)

    Amirhoseiny, Maryam; Zandi, Majid; Mosayyebi, Abolghasem; Khademian, Mehrzad

    2016-01-01

    In this work, electrochemical double layer supercapacitors were fabricated using multiwalled carbon nanotube (MWCNT) composite microfilm as electrode. To improve the electrochemical properties, MWCNTs were functionalized with -COOH by acid treatments. CNT/PVA films have been deposited on different current collectors by spin coating to drastically enhance the electrode performance. Electrode fabrication involved various stages preparing of the CNT composite, and coating of the CNT/PVA paste on different substrates which also served as current collector. Al, Ni and graphite were used and compared as current collectors. The surface morphology of the fabricated electrodes was investigated with scanning electrode microscopy (SEM). Overall cell performance was evaluated with a multi-channel potentiostat/galvanostat analyzer. Each supercapacitor cell was subjected to charge-discharge cycling study at different current rates from 0.2Ag-1 to 1Ag-1. The results showed that graphite-based electrodes offer advantages of significantly higher conductivity and superior capacitive behavior compared to thin film electrodes formed on Ni and Al current collectors. The specific capacitance of graphite based electrode is found to be 29Fg-1.

  15. Amperometric creatinine biosensor based on covalently coimmobilized enzymes onto carboxylated multiwalled carbon nanotubes/polyaniline composite film.

    PubMed

    Yadav, Sandeep; Kumar, Ashok; Pundir, C S

    2011-12-15

    A mixture of commercial creatinine amidohydrolase (CA), creatine amidinohydrolase (CI), and sarcosine oxidase (SO) was coimmobilized covalently via N-ethyl-N'-(3-dimethylaminopropyl) carbodiimide (EDC) and N-hydroxy succinimide (NHS) chemistry onto carboxylated multiwalled carbon nanotube (c-MWCNT)/polyaniline (PANI) nanocomposite film electrodeposited over the surface of a platinum (Pt) electrode. A creatinine biosensor was fabricated using enzyme/c-MWCNT/PANI/Pt as working electrode, Ag/AgCl as reference electrode, and Pt wire as auxiliary electrode connected through potentiostat. The enzyme electrode was characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, and electrochemical impedance spectroscopy (EIS). The biosensor detected creatinine levels as low as 0.1 μM, estimated at a signal-to-noise ratio of 3, within 5s at pH 7.5 and 35°C. The optimized biosensor showed a linear response range of 10 to 750 μM creatinine with sensitivity of 40 μA/mM/cm(2). The fabricated biosensor was successfully employed for determination of creatinine in human serum. The biosensor showed only 15% loss in its initial response after 180 days when stored at 4°C. PMID:21906581

  16. Amperometric determination of xanthine in fish meat by zinc oxide nanoparticle/chitosan/multiwalled carbon nanotube/polyaniline composite film bound xanthine oxidase.

    PubMed

    Devi, Rooma; Yadav, Sandeep; Pundir, C S

    2012-02-01

    Xanthine oxidase (XOD) was immobilized on a composite film of zinc oxide nanoparticle/chitosan/carboxylated multiwalled carbon nanotube/polyaniline (ZnO-NP/CHIT/c-MWCNT/PANI) electrodeposited over the surface of a platinum (Pt) electrode. A xanthine biosensor was fabricated using XOD/ZnO-NP/CHIT/c-MWCNT/PANI/Pt as working electrode, Ag/AgCl as reference electrode and Pt wire as auxiliary electrode connected through a potentiostat. The ZnO-NPs were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM), and the enzyme electrode was characterized by cyclic voltammetry, scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy and electrochemical impedance spectroscopy (EIS). The biosensor showed optimum response within 4 s at 0.5 V potential, pH 7.0, 35 °C and linear range 0.1-100 μM with a detection limit of 0.1 μM. The enzyme electrode was employed for determination of xanthine in fish meat during storage. The electrode lost 30% of its initial activity after 80 uses over one month, when stored at 4 °C. PMID:22135777

  17. Nucleation and growth in electrodeposition of thin copper films on pyrolytic graphite

    SciTech Connect

    Kinaci, F.S.; Muller, R.H.

    1992-05-01

    Electrodeposition of Cu on graphite electrodes was studied, with emphasis on nucleation. Various ex-situ and in-situ methods were investigated for determining the number density of nuclei. Two direct methods were studied (scanning electron microscopy and scanning tunneling microscopy); indirect determinations included Raman spectroscopy and analysis of potentiostatic current transients. Though some of the techniques correctly predicted the nucleation densities under special conditions, SEM was the most reliable tool. The large scatter in the data necessitated steps to minimize this effect. To electrodeposit Cu on graphite, a nucleation overpotential of 250 mV was measured with cyclic voltammetry; such a large overpotential does not occur on a Pt or on a Cu-covered graphite electrode. The deposition potential is the dominant parameter governing nucleation density. There is a sharp increase in the nucleation density with applied potential. Cu can be deposited on highly oriented pyrolytic graphite only between the nucleation overpotential and the hydrogen evolution potential. To increase the Cu nucleation density, while avoiding excessive H evolution, a double pulse potential technique was used; nucleation densities on the order of 10{sup 10} nuclei/cm{sup 2} were achieved. The use of inhibitors (PVA, benzotriazole) was also investigated. Deposition on conducting polymer electrodes was also studied; initial results with polyaniline show promise. 57 figs, 6 tabs, refs. (DLC)

  18. Passivation Dynamics in the Anisotropic Deposition and Stripping of Bulk Magnesium Electrodes During Electrochemical Cycling.

    PubMed

    Wetzel, David J; Malone, Marvin A; Haasch, Richard T; Meng, Yifei; Vieker, Henning; Hahn, Nathan T; Gölzhäuser, Armin; Zuo, Jian-Min; Zavadil, Kevin R; Gewirth, Andrew A; Nuzzo, Ralph G

    2015-08-26

    Although rechargeable magnesium (Mg) batteries show promise for use as a next generation technology for high-density energy storage, little is known about the Mg anode solid electrolyte interphase and its implications for the performance and durability of a Mg-based battery. We explore in this report passivation effects engendered during the electrochemical cycling of a bulk Mg anode, characterizing their influences during metal deposition and dissolution in a simple, nonaqueous, Grignard electrolyte solution (ethylmagnesium bromide, EtMgBr, in tetrahydrofuran). Scanning electron microscopy images of Mg foil working electrodes after electrochemical polarization to dissolution potentials show the formation of corrosion pits. The pit densities so evidenced are markedly potential-dependent. When the Mg working electrode is cycled both potentiostatically and galvanostatically in EtMgBr these pits, formed due to passive layer breakdown, act as the foci for subsequent electrochemical activity. Detailed microscopy, diffraction, and spectroscopic data show that further passivation and corrosion results in the anisotropic stripping of the Mg {0001} plane, leaving thin oxide-comprising passivated side wall structures that demark the {0001} fiber texture of the etched Mg grains. Upon long-term cycling, oxide side walls formed due to the pronounced crystallographic anisotropy of the anodic stripping processes, leading to complex overlay anisotropic, columnar structures, exceeding 50 μm in height. The passive responses mediating the growth of these structures appear to be an intrinsic feature of the electrochemical growth and dissolution of Mg using this electrolyte. PMID:26258957

  19. A new electrochemical sensor for OH radicals detection.

    PubMed

    Gualandi, Isacco; Tonelli, Domenica

    2013-10-15

    A new, cheap modified electrode for indirect detection of OH radical is described. A glassy carbon (GC) electrode was modified with a polyphenol film prepared by oxidative potentiostatic electropolymerization of 0.05 M phenol in 1M H2SO4. The film having a thickness of ~10nm perfectly covered the GC surface and inhibited the charge transfer of many redox species. The degradation of the polyphenol film, that was induced by OH radicals generated by Fenton reaction or by H2O2 photolysis, is the analytical signal and it was evaluated by cyclic voltammetry and chronoamperometry using the redox probe Ru(NH3)6(3+). Some simulations of the kinetics of the reactions occurring in the solution bulk and near the electrode surface were carried out to fully understand the processes that lead to the analytical signal. The modified electrode was used to evaluate the performances of different TiO2-based photocatalysts and the results were successfully compared with those obtained from a traditional HPLC method that is based on the determination of the hydroxylation products of salicylic acid. PMID:24054662

  20. Electrochemical oxidation of tramadol in low-salinity reverse osmosis concentrates using boron-doped diamond anodes.

    PubMed

    Lütke Eversloh, Christian; Schulz, Manoj; Wagner, Manfred; Ternes, Thomas A

    2015-04-01

    The electrochemical treatment of low-salinity reverse osmosis (RO) concentrates was investigated using tramadol (100 μM) as a model substance for persistent organic contaminants. Galvanostatic degradation experiments using boron-doped diamond electrodes at different applied currents were conducted in RO concentrates as well as in ultra-pure water containing either sodium chloride or sodium sulfate. Kinetic investigations revealed a significant influence of in-situ generated active chlorine besides direct anodic oxidation. Therefore, tramadol concentrations decreased more rapidly at elevated chloride content. Nevertheless, reduction of total organic carbon (TOC) was found to be comparatively low, demonstrating that transformation rather than mineralization was taking place. Early stage product formation could be attributed to both direct and indirect processes, including demethylation, hydroxylation, dehydration, oxidative aromatic ring cleavage and halogenation reactions. The latter led to various halogenated derivatives and resulted in AOX (adsorbable organic halogens) formation in the lower mg/L-range depending on the treatment conditions. Characterisation of transformation products (TPs) was achieved via MS(n) experiments and additional NMR measurements. Based on identification and quantification of the main TPs in different matrices and on additional potentiostatic electrolysis, a transformation pathway was proposed. PMID:25660808

  1. Passivation Behavior of Ultrafine-Grained Pure Copper Fabricated by Accumulative Roll Bonding (ARB) Process

    NASA Astrophysics Data System (ADS)

    Fattah-alhosseini, Arash; Imantalab, Omid

    2016-01-01

    In this study, passivation behavior of ultrafine-grained (UFG) pure copper fabricated by ARB process in 0.01 M borax solution has been investigated. Before any electrochemical measurements, evaluation of microstructure was obtained by transmission electron microscopy (TEM). TEM observations revealed that with increasing the number of ARB passes, the grain size of specimens decrease. Also, TEM images showed that UFGs with average size of below 100 nm appeared after 7 passes of ARB. To investigate the passivation behavior of the specimens, electrochemical impedance spectroscopy (EIS) and Mott-Schottky analysis was carried out. For this purpose, three potentials within the passive region were chosen for potentiostatic passive film growth. EIS results showed that both passive film and charge-transfer resistance increases with increasing the number of ARB passes. Moreover, Mott-Schottky analysis revealed that with increasing the number of ARB passes, the acceptor density of the passive films decreased. In conclusion, increasing the number of ARB passes offers better conditions for forming the passive films with higher protection behavior, due to the growth of a much thicker and less defective films.

  2. Role of the electrolyte in cathodic lead dioxide reduction

    SciTech Connect

    Lyamina, L.I.; Gorbunova, K.M.; Tarasova, N.I.

    1985-09-01

    The electrolyte composition and particularly the anions are thought to be important in cathodic lead dioxide reduction. Data are reported for the process in 0.1 M Na/sub 2/B/sub 4/O/sub 7/, Na/sub 2/HPO/sub 4/, KOH, and KC1 solution and in 0.3 M K/sub 2/SO/sub 4/ solution. Deposits of alpha-PbO/sub 2/ were produced electrolytically on nickel. The potentials are reported on the hydrogen scale. The electrochemical behavior of lead dioxide in said solutions was evaluated from charging curves and from potentiodynamic curves obtained with a P-5848 potentiostat. The first stage of lead dioxide reduction in all solutions results in the formation of an intermediate oxide having the composition of PbO/sub 1/ /sub 43/ to PbO/sub 1/ /sub 24/. The second stage (reduction of the intermediate oxide to metallic lead) depends on the nature of the electrolyte. An examination of the results obtained action of lead dioxide with the electrophilic component increases in the order of KOH yields KC1 yields Na/sub 2/B/sub 4/O/sub 7/ yields Na/sub 2/HPO/sub 4/ yields K/sub 2/SO/sub 4/.

  3. Enhanced electrocatalytic activity of the Au-electrodeposited Pt nanoparticles-coated conducting oxide for the quantum dot-sensitized solar cells

    NASA Astrophysics Data System (ADS)

    Yoon, Yeung-Pil; Kim, Jae-Hong; Kang, Soon-Hyung; Kim, Hyunsoo; Choi, Chel-Jong; Kim, Kyong-Kook; Ahn, Kwang-Soon

    2014-08-01

    Au was electrodeposited potentiostatically at 0.3 V for 5 min on nanoporous Pt nanoparticle-coated F-doped SnO2 (FTO/Pt) substrates. For comparison, Au-electrodeposited FTO (FTO/Au) and Au-uncoated FTO/Pt were prepared. FTO/Au showed large-sized Au clusters dispersed sparsely over FTO, which resulted in lower electrocatalytic activity than FTO/Pt. In contrast, FTO/Pt exhibited poor stability unlike FTO/Au due to poisoning by the adsorption of sulfur species. The Au-electrodeposited FTO/Pt (FTO/Pt/Au) consisted of small Au clusters deposited over the entire area of Pt due to the effective Au nucleation provided by nanoporous metallic Pt. FTO/Pt/Au exhibited enhanced electrocatalytic activity and excellent stability because the small Au particles well-dispersed over the nanoporous metallic Pt network provided numerous electrochemical reaction sites, and the Pt surface was not exposed to the electrolyte. When FTO/Pt/Au was used as the counter electrode (CE) of a quantum dot-sensitized solar cell, the significantly enhanced electrocatalytic activity of the FTO/Pt/Au CE facilitated the reduction reaction of Sn2- + 2e- (CE) → Sn-12- + S2- at the CE/electrolyte interface, resulting in a significantly hindered recombination reaction, Sn2- + 2e- (TiO2 in the photoanode) → Sn-12- + S2-, and significantly improved overall energy conversion efficiency.

  4. Delayed feedback induced multirhythmicity in the oscillatory electrodissolution of copper

    NASA Astrophysics Data System (ADS)

    Nagy, Timea; Verner, Erika; Gáspár, Vilmos; Kori, Hiroshi; Kiss, István Z.

    2015-06-01

    Occurrence of bi- and trirhythmicities (coexistence of two or three stable limit cycles, respectively, with distinctly different periods) has been studied experimentally by applying delayed feedback control to the copper-phosphoric acid electrochemical system oscillating close to a Hopf bifurcation point under potentiostatic condition. The oscillating electrode potential is delayed by τ and the difference between the present and delayed values is fed back to the circuit potential with a feedback gain K. The experiments were performed by determining the period of current oscillations T as a function of (both increasing and decreasing) τ at several fixed values of K. With small delay times, the period exhibits a sinusoidal type dependence on τ. However, with relatively large delays (typically τ ≫ T) for each feedback gain K, there exists a critical delay τcrit above which birhythmicity emerges. The experiments show that for weak feedback, Kτcrit is approximately constant. At very large delays, the dynamics becomes even more complex, and trirhythmicity could be observed. Results of numerical simulations based on a general kinetic model for metal electrodissolution were consistent with the experimental observations. The experimental and numerical results are also interpreted by using a phase model; the model parameters can be obtained from experimental data measured at small delay times. Analytical solutions to the phase model quantitatively predict the parameter regions for the appearance of birhythmicity in the experiments, and explain the almost constant value of Kτcrit for weak feedback.

  5. The effect of expanders on lead-sulphate formation and reduction

    NASA Astrophysics Data System (ADS)

    Francia, Carlotta; Maja, Mario; Spinelli, Paolo

    The influence of some organic expanders on the formation of lead-sulphate has been studied by means of potentiostatic transients. The experimental data have been discussed according to the theories which have been proposed in the literature for the electro-crystallisation of lead-sulphate and lead. The discussion of the data obtained confirms the inhibiting effect of the expanders on lead sulphation. In fact, the tests showed that, when the expanders are added to the electrolyte, a longer time is required to reach the current maximum of the i( t) curve and a reduction of its intensity. According to the theoretical interpretation, this finding indicates a decreasing of the kinetic constant of the solid state process. The analysis of the i( t) transients obtained during the sulphate reduction revealed an influence of expanders only when the sulphate layers has been formed in their presence. Thus, it seems that the adsorption of the organic expanders on lead is of primary importance for their action while adsorption on lead-sulphate appears to be negligible.

  6. The anodic behavior of iron in hydrogen sulfide solutions

    SciTech Connect

    Pound, B.G. ); Wright, G.A.; Sharp, R.M. . Dept. of Chemistry)

    1989-05-01

    The anodic behavior of iron in 0.032 mol . L/sup -1/ NaCl/0.003 mol . L/sup -1/ NaHCO/sub 3/ and 1 mol . L/sup -1/ Na/sub 2/SO/sub 4//0.003 mol . L/sup -1/ NaHCO/sub 3/ solutions containing 0.05 mol . L/sup -1/ H/sub 2/S at ambient temperature was studied using cyclic voltammetry and the potentiostatic technique. In both solutions, a nonprotective film of mackinawite (Fe/sub 1+chi/S) was formed on the iron, but the film growth kinetics differ for the two solutions. The film growth in chloride solutions does not appear to follow a conventional type of model for multilayer fils whereas the formation of the film in sulfate solutions can be represented in terms of a pre-resistance model. At more anodic potentials, the mackinawite is oxidized to a higher sulfide, possibly pyrite (FeS/sub 2/), as suggested from a comparison of the anodic and cathodic peak potentials with the equilibrium potential. The formation of the higher sulfide(s) in the chloride solution appears to follow a similar film growth mechanism to that for mackinawite, whereas it is not clear whether this is the case for the sulfate solution.

  7. Coatings on NiTi Alloy

    NASA Astrophysics Data System (ADS)

    Kei, C. C.; Yu, Y. S.; Racek, J.; Vokoun, D.; Šittner, P.

    2014-07-01

    Atomic layer deposition is introduced as a method suitable for preparation of Al2O3 layers on the surface of NiTi medical devices such as stents because of the excellent thickness control and conformal protective coating on complex structures. The corrosion properties of NiTi plates with Al2O3 coatings of various thicknesses in an environment similar to that occurring in the human body were studied using open circuit potential, potentiostatic electrochemical impedance spectroscopy, and cyclic polarization tests. It shows that the layer thickness plays a key role in the inhibition of corrosion. The thinner layers are more diffuse and make it easier for anodic reaction of passive NiTi with protective TiO2 underneath of Al2O3, while the thicker layers have the barrier effect with local pores initiating pitting corrosion. The results of our electrochemical experiments consistently show that corrosion properties of thick Al2O3 coatings on NiTi plate are inferior compared to the thin layers.

  8. Using anodic aluminum oxide templates and electrochemical method to deposit BiSbTe-based thermoelectric nanowires

    NASA Astrophysics Data System (ADS)

    Kuo, Hsin-Hui; Kuo, Chin-Guo; Yen, Chia-Ying; Yang, Cheng-Fu

    2014-02-01

    In this study, the cyclic voltammetry method was first used to find the reduced voltages and anodic peaks of Bi3+, Sb3+, and Te4+ ions as the judgments for the growth of the (Bi,Sb)2 - x Te3 + x -based materials. Ethylene glycol (C2H6O2) was used as a solvent, and 0.3 M potassium iodide (KI) was used to improve the conductivity of the solution. Two different electrolyte formulas were first used: (a) 0.01 M Bi(NO3)3-5H2O, 0.01 M SbCl3, and 0.01 M TeCl4 and (b) 0.015 M Bi(NO3)3-5H2O, 0.005 M SbCl3, and 0.0075 M TeCl4. The potentiostatic deposition process was first used to find the effect of reduced voltage on the variation of compositions of the (Bi,Sb)2 - x Te3 + x -based materials. After finding the better reduced voltage, 0.01 M Bi(NO3)3-5H2O, 0.01 M SbCl3, and 0.01 M TeCl4 were used as the electrolyte formula. The pulse deposition process was successfully used to control the composition of the (Bi,Sb)2 - x Te3 + x -based materials and grow the nanowires in anodic aluminum oxide (AAO) templates.

  9. Effects of anodization growth of TiO2-nanotube array membrane on photo-conversion efficiency of dye-sensitized solar cell

    NASA Astrophysics Data System (ADS)

    Park, Min-Woo; Chun, Ki-Young

    2009-03-01

    Membranes of TiO2 nanotube(NT) arrays were grown by potentiostatic anodic oxidation in an ethylene glycol electrolyte with small addition of H2O and NH4F. Ti metal plate with a thickness of 0.1 mm was completely converted into ≈0.2 mm-thick TiO2 NT membrane for 24 to 96 h of anodization. Stacked NTs in membrane were separated into individual NT from the neighboring NTs as anodization continues up to 96 h. As-fabricated membrane of NTs were mechanically grinded to yield fine NT particles for the photoanode application to dye-sensitized solar cells (DSCs), in replacement of conventional TiO2 particles. Photo-conversion efficiency of the DSC using TiO2 crystalline NT particles is varying from 2.22% to 5.03%. Fine TiO2 NT particles can increase dye attachment due to high surface to volume ratio.

  10. Effect of Fluid Flow on Zinc Electrodeposits from Acid Chloride Electrolytes. M.S. Thesis

    NASA Technical Reports Server (NTRS)

    Abdelmassir, A. A.

    1982-01-01

    Zinc was deposited potentiostatically from acid chloride baths. Once bath chemistry and electrochemistry were controlled, the study was focused on convective mass transfer at horizontal electrodes and its effect on cell performance. A laser schlieren imaging technique allowed in situ observations of flow patterns and their correlation with current transients. Convection was turbulent and mass transfer as a function of Rayleigh number was well correlated by: Sh = 0.14 R to the 1/3 power. Similarly, convection initiation time was correlated by DT/d squared = 38 Ra to the -2/3 power. Time scale of fluctuations was about half the initiation time. Taking the boundary layer thickness as a characteristic length, a critical Rayleigh number for the onset of convection was deduced: Ra sub CR = 5000. Placing the anode on the top of the cathode completely changed the flow pattern but kept the I-t curves identical whereas the use of a cathode grid doubled the limiting current. A well defined plateau in the current voltage curves suggested that hydrogen evolution has been successfully inhibited. Finally, long time deposition showed that convection at horizontal electrodes increased the induction time for dentrite growth by at least a factor of 2 with respect to a vertical wire.

  11. Study on Electro-polymerization Nano-micro Wiring System Imitating Axonal Growth of Artificial Neurons towards Machine Learning

    NASA Astrophysics Data System (ADS)

    Dang, Nguyen Tuan; Akai-Kasada, Megumi; Asai, Tetsuya; Saito, Akira; Kuwahara, Yuji; Hokkaido University Collaboration

    2015-03-01

    Machine learning using the artificial neuron network research is supposed to be the best way to understand how the human brain trains itself to process information. In this study, we have successfully developed the programs using supervised machine learning algorithm. However, these supervised learning processes for the neuron network required the very strong computing configuration. Derivation from the necessity of increasing in computing ability and in reduction of power consumption, accelerator circuits become critical. To develop such accelerator circuits using supervised machine learning algorithm, conducting polymer micro/nanowires growing process was realized and applied as a synaptic weigh controller. In this work, high conductivity Polypyrrole (PPy) and Poly (3, 4 - ethylenedioxythiophene) PEDOT wires were potentiostatically grown crosslinking the designated electrodes, which were prefabricated by lithography, when appropriate square wave AC voltage and appropriate frequency were applied. Micro/nanowire growing process emulated the neurotransmitter release process of synapses inside a biological neuron and wire's resistance variation during the growing process was preferred to as the variation of synaptic weigh in machine learning algorithm. In a cooperation with Graduate School of Information Science and Technology, Hokkaido University.

  12. 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. PMID:25897977

  13. Electrochemical removal of hydrogen atoms in Mg-doped GaN epitaxial layers

    NASA Astrophysics Data System (ADS)

    Lee, June Key; Hyeon, Gil Yong; Tawfik, Wael Z.; Choi, Hee Seok; Ryu, Sang-Wan; Jeong, Tak; Jung, Eunjin; Kim, Hyunsoo

    2015-05-01

    Hydrogen atoms inside of an Mg-doped GaN epitaxial layer were effectively removed by the electrochemical potentiostatic activation (EPA) method. The role of hydrogen was investigated in terms of the device performance of light-emitting diodes (LEDs). The effect of the main process parameters for EPA such as solution type, voltage, and time was studied and optimized for application to LED fabrication. In optimized conditions, the light output of 385-nm LEDs was improved by about 26% at 30 mA, which was caused by the reduction of the hydrogen concentration by ˜35%. Further removal of hydrogen seems to be involved in the breaking of Ga-H bonds that passivate the nitrogen vacancies. An EPA process with high voltage breaks not only Mg-H bonds that generate hole carriers but also Ga-H bonds that generate electron carriers, thus causing compensation that impedes the practical increase of hole concentration, regardless of the drastic removal of hydrogen atoms. A decrease in hydrogen concentration affects the current-voltage characteristics, reducing the reverse current by about one order and altering the forward current behavior in the low voltage region.

  14. Enhanced durability of a proton conducting oxide fuel cell with a purified yttrium-doped barium zirconate-cerate electrolyte

    NASA Astrophysics Data System (ADS)

    Hakim, Muhammad; Yoo, Chung-Yul; Joo, Jong Hoon; Yu, Ji Haeng

    2015-03-01

    The aim of this study is to investigate the effect of yttrium-doped barium zirconate-cerate (BaZr0.3Ce0.5Y0.2O3-?, BZCY) refinement on cell stability under operational fuel cell conditions. For this purpose, anode-supported cells, comprised of a nickel oxide (NiO)-BZCY anode, a BZCY electrolyte, and a BZCY-La0.6Sr0.4Co0.2Fe0.8O3-? composite cathode are successfully prepared with refined or as-calcined BZCY powder. The long-term fuel cell performance is evaluated under a potentiostatic measurement at 600 C. The cell with the refined BZCY electrolyte shows a modest power density of 47 mW cm-2 at a 600 C operating temperature over 480 h without any significant performance loss, whereas the cell with the as-calcined BZCY electrolyte displays a rapid degradation of cell performance over 110 h. A post-testing analysis of the cell with the refined BZCY does not reveal any evidence of delamination resulting from electrolyte surface decomposition. These results demonstrate that the refinement process significantly enhances the chemical stability of BZCY-based proton conducting fuel cells, which produce a high content of water vapor on the cathode side.

  15. Passivation dynamics in the anisotropic deposition and stripping of bulk magnesium electrodes during electrochemical cycling

    SciTech Connect

    Wetzel, David J.; Malone, Marvin A.; Haasch, Richard T.; Meng, Yifei; Vieker, Henning; Hahn, Nathan; Golzhauser, Armin; Zuo, Jian-Min; Zavadil, Kevin R.; Gewirth, Andrew A.; Nuzzo, Ralph G.

    2015-08-10

    Rechargeable magnesium (Mg) batteries show promise for use as a next generation technology for high-density energy storage, though little is known about the Mg anode solid electrolyte interphase and its implications for the performance and durability of a Mg-based battery. We explore in this report passivation effects engendered during the electrochemical cycling of a bulk Mg anode, characterizing their influences during metal deposition and dissolution in a simple, nonaqueous, Grignard electrolyte solution (ethylmagnesium bromide, EtMgBr, in tetrahydrofuran). Scanning electron microscopy images of Mg foil working electrodes after electrochemical polarization to dissolution potentials show the formation of corrosion pits. The pit densities so evidenced are markedly potential-dependent. When the Mg working electrode is cycled both potentiostatically and galvanostatically in EtMgBr these pits, formed due to passive layer breakdown, act as the foci for subsequent electrochemical activity. Detailed microscopy, diffraction, and spectroscopic data show that further passivation and corrosion results in the anisotropic stripping of the Mg {0001} plane, leaving thin oxide-comprising passivated side wall structures that demark the {0001} fiber texture of the etched Mg grains. Upon long-term cycling, oxide side walls formed due to the pronounced crystallographic anisotropy of the anodic stripping processes, leading to complex overlay anisotropic, columnar structures, exceeding 50 μm in height. Finally, the passive responses mediating the growth of these structures appear to be an intrinsic feature of the electrochemical growth and dissolution of Mg using this electrolyte.

  16. New Secondary Batteries Utilizing Electronically Conductive Polypyrrole Cathode. Ph.D. Thesis

    NASA Technical Reports Server (NTRS)

    Yeu, Taewhan

    1991-01-01

    To gain a better understanding of the dynamic behavior in electronically conducting polypyrroles and to provide guidance toward designs of new secondary batteries based on these polymers, two mathematical models are developed; one for the potentiostatically controlled switching behavior of polypyrrole film, and one for the galvanostatically controlled charge/discharge behavior of lithium/polypyrrole secondary battery cell. The first model is used to predict the profiles of electrolyte concentrations, charge states, and electrochemical potentials within the thin polypyrrole film during switching process as functions of applied potential and position. Thus, the detailed mechanisms of charge transport and electrochemical reaction can be understood. Sensitivity analysis is performed for independent parameters, describing the physical and electrochemical characteristic of polypyrrole film, to verify their influences on the model performance. The values of independent parameters are estimated by comparing model predictions with experimental data obtained from identical conditions. The second model is used to predict the profiles of electrolyte concentrations, charge state, and electrochemical potentials within the battery system during charge and discharge processes as functions of time and position. Energy and power densities are estimated from model predictions and compared with existing battery systems. The independent design criteria on the charge and discharge performance of the cell are provided by studying the effects of design parameters.

  17. High temperature oxygen transport and electrochemical behavior of YBa[sub 2]Cu[sub 3]O[sub x

    SciTech Connect

    Guer, T.M. . Dept. of Materials Science and Engineering); Huggins, R.A. )

    1993-07-01

    Over the last several decades, solid oxide electrolytes based on stabilized zirconia have found extensive use in applications such as oxygen sensors, solid oxide fuel cells, oxygen pumps, electrocatalytic reactors, and electrochemically driven oxygen separation membranes. In this preliminary study, the high temperature oxygen transport and electrochemical behavior of YBa[sub 2]Cu[sub 3]O[sub x] was evaluated in a solid-state electrochemical cell employing a yttria-stabilized zirconia (YSZ) solid electrolyte. The oxygen chemical diffusion coefficient was measured by a solid-state potentiostatic step technique and found to be 5 x 10[sup [minus]8] cm[sup 2]/s at 800 C. The dc polarization behavior of YBa[sub 2]Cu[sub 3]O[sub x] electrodes deposited on YSZ electrolyte was governed primarily by an ohmic process in oxygen, air, and He environments in both the anodic and cathodic directions. The frequency dispersion of the electrochemical response, obtained by ac impedance spectroscopy showed two depressed circular arcs in complex plane plots that are offset from the origin, indicative of a resistive path in the equivalent circuit model at high frequencies. It is proposed that the YBa[sub 2]Cu[sub 3]O[sub x] electrode poses the major impedance to the overall rate and dominates the electrochemical performance of the cell.

  18. Protein-Support Interactions for Rationally Designed Bilirubin Oxidase Based Cathode: A Computational Study.

    PubMed

    Matanovic, Ivana; Babanova, Sofia; Chavez, Madelaine Seow; Atanassov, Plamen

    2016-04-21

    An example of biocathode based on bilirubin oxidase (BOx) was used to demonstrate how density functional theory can be combined with docking simulations in order to study the interface interactions between the enzyme and specifically designed electrode surface. The electrode surface was modified through the adsorption of bilirubin, the natural substrate for BOx, and the prepared electrode was electrochemically characterized using potentiostatic measurements. The experimentally determined current densities showed that the presence of bilirubin led to significant improvement of the cathode operation. On the basis of the computationally calculated binding energies of bilirubin to the graphene support and BOx and the analysis of the positioning of bilirubin relative to the support and T1 Cu atom of the enzyme, we hypothesize that the bilirubin serves as a geometric and electronic extension of the support. The computational results further confirm that the modification of the electrode surface with bilirubin provides an optimal orientation of BOx toward the support but also show that bilirubin facilitates the interfacial electron transfer by decreasing the distance between the electrode surface and the T1 Cu atom. PMID:27015361

  19. Marine phototrophic consortia transfer electrons to electrodes in response to reductive stress.

    PubMed

    Darus, Libertus; Ledezma, Pablo; Keller, Jürg; Freguia, Stefano

    2016-03-01

    This work studies how extracellular electron transfer (EET) from cyanobacteria-dominated marine microbial biofilms to solid electrodes is affected by the availability of inorganic carbon (Ci). The EET was recorded chronoamperometrically in the form of electrical current by a potentiostat in two identical photo-electrochemical cells using carbon electrodes poised at a potential of +0.6 V versus standard hydrogen electrode under 12/12 h illumination/dark cycles. The Ci was supplied by the addition of NaHCO3 to the medium and/or by sparging CO2 gas. At high Ci conditions, EET from the microbial biofilm to the electrodes was observed only during the dark phase, indicating the occurrence of a form of night-time respiration that can use insoluble electrodes as the terminal electron acceptor. At low or no Ci conditions, however, EET also occurred during illumination suggesting that, in the absence of their natural electron acceptor, some cyanobacteria are able to utilise solid electrodes as an electron sink. This may be a natural survival mechanism for cyanobacteria to maintain redox balance in environments with limiting CO2 and/or high light intensity. PMID:26407568

  20. Effects of Osseointegration by Bone Morphogenetic Protein-2 on Titanium Implants In Vitro and In Vivo.

    PubMed

    Teng, Fu-Yuan; Chen, Wen-Cheng; Wang, Yin-Lai; Hung, Chun-Cheng; Tseng, Chun-Chieh

    2016-01-01

    This study designed a biomimetic implant for reducing healing time and achieving early osseointegration to create an active surface. Bone morphogenetic protein-2 (BMP-2) is a strong regulator protein in osteogenic pathways. Due to hardly maintaining BMP-2 biological function and specificity, BMP-2 efficient delivery on implant surfaces is the main challenge for the clinic application. In this study, a novel method for synthesizing functionalized silane film for superior modification with BMP-2 on titanium surfaces is proposed. Three groups were compared with and without BMP-2 on modified titanium surfaces in vitro and in vivo: mechanical grinding; electrochemical modification through potentiostatic anodization (ECH); and sandblasting, alkali heating, and etching (SMART). Cell tests indicated that the ECH and SMART groups with BMP-2 markedly promoted D1 cell activity and differentiation compared with the groups without BMP-2. Moreover, the SMART group with a BMP-2 surface markedly promoted early alkaline phosphatase expression in the D1 cells compared with the other surface groups. Compared with these groups in vivo, SMART silaning with BMP-2 showed superior bone quality and created contact areas between implant and surrounding bones. The SMART group with BMP-2 could promote cell mineralization in vitro and osseointegration in vivo, indicating potential clinical use. PMID:26977141

  1. Relevance of an electrochemical process prior to a biological treatment for the removal of an organophosphorous pesticide, phosmet.

    PubMed

    Salles, Nara Alonso; Fourcade, Florence; Geneste, Florence; Floner, Didier; Amrane, Abdeltif

    2010-09-15

    The aim of this study was to examine the feasibility of coupling an electrochemical pre-treatment with a biological step in order to degrade phosmet, an organophosphorous pesticide. Preliminary biodegradation experiments showed that the target molecule was not assimilated by activated sludge. The pre-treatment consisted of potentiostatic electrolysis (-1.3 V/SCE) in a flow cell. After only one pass (1 mL min(-1)), cyclic voltammetry with a vitreous carbon electrode showed a total phosmet reduction in neutral medium confirmed by thin layer chromatography, which also highlighted the presence of several by-products. H NMR spectra of the main by-product showed the absence of the aromatic ring, only the phosphorus part of phosmet has been identified and phosmet-oxon, a very toxic derivative, was not formed. Lower toxicity and higher biodegradability characterized the electrolyzed solution, EC(50) value increased from 7% to 58% and BOD(5) value increased from 4 to 9 mg O(2) L(-1) after electrolysis leading to an increase of the BOD(5) on COD ratio from 0.19 to 0.42 (limit of biodegradability, 0.4). These encouraging results were confirmed during activated sludge culture since an almost total mineralization of the electrolyzed solution was recorded (97%), confirming the feasibility of the proposed coupled process. PMID:20538412

  2. The open-circuit ennoblement of alloy C-22 and other Ni-Cr-Mo alloys

    NASA Astrophysics Data System (ADS)

    Lloydis, A. C.; Noël, J. J.; Shoesmith, D. W.; McIntyre, N. S.

    2005-01-01

    The open-circuit corrosion and anodic oxidation behavior of the C-series of Ni-Cr-Mo alloys (C-4, C-276, C-2000, and C-22) and alloy 625 have been studied at 25°C and 75°C in 1.0 mol·L-1 NaCl+1.0 mol·L-1 H2SO4. A combination of open-circuit potential, potentiostatic polarization, and electrochemical impedance spectroscopy were employed in the study. The composition of the films formed was determined by x-ray photoelectron spectroscopy and time-of-flight secondary ion mass spectrometry. Passive oxide film resistances increase and defect oxide film concentrations decrease as films thicken and chromium and molybdenum segregate to the alloy/oxide and oxide/solution interfaces, respectively. The high-chromium alloys exhibit higher film resistances and lower film defect concentrations consistent with the more positive potentials observed on these alloys. The results show that the observed ennoblement in corrosion potentials with time is coupled to the Cr/Mo segregation process and the suppression of defect injection at the alloy/oxide interface. By all measures, C-22 exhibited the best passive properties.

  3. A Portable Luminometer with a Disposable Electrochemiluminescent Biosensor for Lactate Determination

    PubMed Central

    Martínez-Olmos, Antonio; Ballesta-Claver, Julio; Palma, Alberto J.; Valencia-Mirón, Maria del Carmen; Capitán-Vallvey, Luis Fermin

    2009-01-01

    A hand-held luminometer for measuring electrochemiluminescence (ECL) for lactate determination and based on one-shot biosensors fabricated using screen-printed electrodes is described. The lactate recognition system is based on lactate oxidase and the transduction system consists of electro-oxidation of luminol, with all the reagents immobilized in a Methocel membrane. The membrane composition and reaction conditions have been optimized to obtain adequate sensitivity. The luminometer is based on a large silicon photodiode as detector and includes a programmable potentiostat to initialize the chemical reaction and signal processing circuitry, designed to acquire a low level photocurrent with offset cancelation, low pass filtering for noise attenuation and adjustable gain up to 1012 V/A. The one-shot biosensor responds to lactate rapidly, with an acquisition time of 2.5 min, obtaining a linear dependence from 8 × 10−6 to 2 × 10−4 M, a detection limit of 2.4 × 10−6 M and a sensor-to-sensor reproducibility (relative standard deviation, RSD) of around 7–10 % at the medium level of the range. PMID:22408475

  4. SEMICONDUCTOR MATERIALS: Effect of bath temperature on the properties of CuInxGa1-x Se2 thin films grown by the electrodeposition technique

    NASA Astrophysics Data System (ADS)

    Jie, Cao; Shengchun, Qu; Kong, Liu; Zhanguo, Wang

    2010-08-01

    Electrodeposition is a promising and low cost method to synthesize CuInx Ga1-x Se2 (CIGS)thin films as an absorber layer for solar cells. The effect of bath temperature on the properties of CIGS thin films was investigated in this paper. CIGS films of 1 μm thickness were electrodeposited potentiostatically from aqueous solution, containing trisodium citrate as a complexing agent, on Mo/glass substrate under a voltage of -0.75 V, and bath temperatures were varied from 20 to 60°C. The effects of bath temperature on the properties of CIGS thin films were characterized by X-ray diffraction (XRD) and scanning electron microscopy. XRD revealed the presence of the CuIni0.7Ga0.3 Se2 phase, the optimal phase for application in solar cells. The grain dimensions and crystallizability increase along with the increase of the bath temperature, and the films become stacked and homogeneous. There were few changes in surface morphology and the composition of the films.

  5. Bioactivity of self-organized TiO2 nanotubes used as surface treatment on Ti biomaterials

    NASA Astrophysics Data System (ADS)

    Souza, M. R.; Reyes, K. M.; Oliveira, N. T. C.; Kuromoto, N. K.; Marino, C. E. B.

    2016-03-01

    Titanium and its alloys are widely used as implants due to their excellent mechanical properties, corrosion resistance and biocompatibility. TiO2 nanotubes have been studied as surface treatment to increase the specific area and to improve osseointegration. However, the thermodynamic stability and bioactivity of these nanostructures must be evaluated. The objective of this research was to obtain nanotubes oxides on Ti6Al4V alloy and to analyze the electrochemical stability in physiological solution at 37 °C and the bioactive response of the biomaterial. The nanotubes were obtained by potentiostatic anodization. The morphology of the oxides was evaluated by scanning electron microscopy. The chemical characterization was analyzed by energy dispersive spectroscopy and x-ray photoelectron spectroscopy techniques. The electrochemical stability was analyzed by open circuit potential (OCP) and the bioactivity by biomimetic test in a simulated body fluid (SBF) solution. The OCP of the nanotubes oxides was shown to be more noble and stable than the compacted oxides. The biomaterial covered with theses oxides showed sealing by Ca and P after 30 d immersion in artificial blood. And after 15 d of immersion in SBF, the hydroxyapatite could be seen on the non-sealed nanotubes. TiO2 nanotube layers could improve the superficial chemical stability and also the osseointegration process.

  6. Preparation of electrodeposited Zn-Ni-B alloy coatings

    NASA Astrophysics Data System (ADS)

    Sakai, Taro; Kamimoto, Yuki; Ichino, Ryoichi

    2016-01-01

    We prepared Zn-Ni-B alloys with high Zn content and high corrosion resistance. The composition of the alloys was controlled by potentiostatic electrolysis. In the electroplating bath, dimethylamineborane was used as the B source. The characterization of the alloys and corrosion resistance evaluation were carried out by X-ray diffraction (XRD) analysis, optical microscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), inductively coupled plasma-atomic emission spectrometry (ICP-AES), Tafel plots, and cyclic corrosion tests. All films were categorized into three groups on the basis of the results of XRD analysis, and it was found by TEM analysis that the Ni-B-type showed an amorphous structure. The Ni-B-type could contain up to 50.6 mol % Zn and showed similar or better anticorrosion properties than the amorphous Ni-B films. In the Ni-B-type, the higher the Zn content, the higher the corrosion resistance. The Zn-Ni-B alloys had almost the same electrochemical corrosion resistance and Zn content as the Zn-Ni-P alloys.

  7. The influence of complexing agent and proteins on the corrosion of stainless steels and their metal components.

    PubMed

    Kocijan, Aleksandra; Milosev, Ingrid; Pihlar, Boris

    2003-01-01

    The present work is devoted to the problem of biodegradation of orthopaedic implants manufactured from stainless steel. In vitro simulations of the biocompatibility of two types of stainless steel, AISI 304 and AISI 316L, and their individual metal components, i.e. iron, chromium, nickel and molybdenum, were carried out in simulated physiological solution (Hank's) containing complexing agents. Knowledge of the effects of the chemical and biological complexing agents, EDTA and proteins, respectively, on the corrosion resistance of a metal should provide a better understanding of the processes occurring in vivo on its surface. The behavior of stainless steels and metal components was studied under open circuit and under potentiostatic conditions. The concentration of dissolved corrosion products in the form of released ions was determined by differential pulse polarography (DPP) and atomic emission spectrometry using inductively coupled plasma (ICP-AES). The composition of solid corrosion products formed on the surface was analyzed by energy dispersive X-ray spectroscopy (EDS) and their morphology was viewed by scanning electron microscopy (SEM). The addition of EDTA and proteins to physiological solution increased the dissolution of pure metals and stainless steels. The effect of particular protein differs on different metals and alloys. PMID:15348541

  8. Electrodeposition of palladium on carbon nanotubes modified nickel foam as an efficient electrocatalyst towards hydrogen peroxide reduction

    NASA Astrophysics Data System (ADS)

    Yang, Fan; Cao, Bo; Tao, Yue; Hu, Miao; Feng, Chengcheng; Wang, Lei; Jiang, Zhao; Cao, Dianxue; Zhang, Ying

    2015-12-01

    In this article, a three-dimensional electrode (Pd-CNT/Ni foam) based on Pd nanoparticles and carbon nanotubes (CNTs) is successfully developed by a simple "dipping and drying" process and a potentiostatic deposition technology for H2O2 reduction in base medium. The composition and structure of Pd-CNT/Ni foam electrode are examined by X-ray diffractometer, scanning electron microscopy, energy-dispersive X-ray spectroscopy, transmission electron microscopy, respectively. The cyclic voltammetry (CV) and chronoamperometry (CA) techniques are applied to determine the electrochemical performance. The electrode exhibits a high catalytic activity for H2O2 electroreduction, and it outperforms Pd/Ni foam electrode without CNT coating. At the reduction potential of -0.8 V, the reduction currents on Pd-CNT/Ni foam electrode can reach 323 mA cm-2, however, it is only 192 mA cm-2 on Pd/Ni foam electrode, which is increased by 68.2%. The impressive electrocatalytic performance is largely attributed to the superior open structure and high electronic conductivity, which allows the high utilization of Pd surfaces and makes the electrode have higher electrochemical activity. These findings may provide the opportunity on preparing binder-free carbon-supported electrode in the application of fuel cells.

  9. Overpotential-Dependent Phase Transformation Pathways

    SciTech Connect

    Y Kao; M Tang; N Meethong; J Bai; W Carter; Y Chiang

    2011-12-31

    An objective in battery development for higher storage energy density is the design of compounds that can accommodate maximum changes in ion concentration over useful electrochemical windows. Not surprisingly, many storage compounds undergo phase transitions in situ, including production of metastable phases. Unique to this environment is the frequent application of electrical over- and underpotentials, which are the electrical analogs to undercooling and superheating. Surprisingly, overpotential effects on phase stability and transformation mechanisms have not been studied in detail. Here we use synchrotron X-ray diffraction performed in situ during potentiostatic and galvanostatic cycling, combined with phase-field modeling, to reveal a remarkable dependence of phase transition pathway on overpotential in the model olivine Li{sub 1-x}FePO{sub 4}. For a sample of particle size {approx}113 nm, at both low (e.g., <20 mV) and high (>75 mV) overpotentials a crystal-to-crystal olivine transformation dominates, whereas at intermediate overpotentials a crystalline-to-amorphous phase transition is preferred. As particle sizes decrease to the nanoscale, amorphization is further emphasized. Implications for battery use and design are considered.

  10. Overpotential-Dependent Phase Transformation Pathways in Lithium Iron Phosphate Battery Electrodes

    SciTech Connect

    Kao, Yu-Hua; Tang, Ming; Meethong, Nonglak; Bai, Jianming; Carter, Craig; Chiang, Yet-Ming

    2010-01-01

    An objective in battery development for higher storage energy density is the design of compounds that can accommodate maximum ion concentration change over useful electrochemical windows. Not surprisingly, many storage compounds undergo phase transitions in-situ, including production of metastable phases. Unique to this environment is the frequent application of electrical over- and underpotentials, which are the electrical analogs to undercooling and superheating. Surprisingly, overpotential effects on phase stability and transformation mechanisms have not been studied in detail. Here we use synchrotron X-ray diffraction performed in-situ during potentiostatic and galvanostatic cycling, combined with phase-field modeling, to reveal a remarkable dependence of phase transition pathway on overpotential in the model olivine Li1-xFePO4. At both low (e.g., <20 mV) and high (>75 mV) overpotentials a crystal-to-crystal olivine transformation is preferred, whereas at intermediate overpotentials a crystalline-to-amorphous phase transition dominates. At nanoscale particle size, amorphization is further emphasized. Implications for battery use and design are considered.

  11. Exploratory development of an electrically rechargeable lithium battery

    NASA Astrophysics Data System (ADS)

    Abraham, K. M.; Goldman, J. L.; Dempsey, M. D.; Holleck, G. L.

    1980-10-01

    The cathodic behavior or V6013 was investigated in rechargeable Li cells of the type, Li/2Me-THF,LiAsF6/V6013,C. Two forms of V6013 were synthesized and characterized. These were a stoichiometric form, i.e., V02.17, and a slightly non-stoichiometric form, i.e., V02.19. Stoichiometric V6013 was prepared by heating requisite quantities of V205 and V powder for 24 hrs. at 650 C. The slightly non-stoichiometric V6013 was prepared by the thermal decomposition of NH4V03 at 450 C. The discharge characteristics of the stoichiometric oxide at 60 C were similar to that of non-stoichiometric oxide at room temperature. The rechargeability of both the oxides were found to be sensitive to the lower voltage cutoff. The safest limits of cycling were 3.0 and 1.9V. Potentiostatic discharges of the oxides between 1.9 and 1.3V revealed a high capacity irreversible reduction process at about 1.6V. Three types of hermetically sealed cells were constructed and tested. In a high capacity (5Ah) prismatic cell utilizing the non-stoichiometric oxide, energy densities of 106 Whr/kg and 190 Whr/DM3 were achieved.

  12. Reduction of CO2 to low carbon alcohols on CuO FCs/Fe2O3 NTs catalyst with photoelectric dual catalytic interfaces.

    PubMed

    Li, Peiqiang; Wang, Huying; Xu, Jinfeng; Jing, Hua; Zhang, Jun; Han, Haixiang; Lu, Fusui

    2013-12-01

    In this paper, the CuO FCs/Fe2O3 NTs catalyst was obtained after Fe2O3 nanotubes (Fe2O3 NTs) were decorated with CuO flower clusters (CuO FCs) by the pulse electrochemical deposition method. The in situ vertically aligned Fe2O3 NTs were prepared on the ferrous substrate by a potentiostatic anodization method. The SEM result showed the volcano-like Fe2O3 NTs were arranged in order and the CuO FCs constituted of flaky CuO distributed on the Fe2O3 NTs surface uniformly. After CuO FCs were loaded on Fe2O3 NTs, the absorption of visible light was enhanced noticeably, and its band gap narrowed to 1.78 eV from 2.03 eV. The conduction band and valence band locating at -0.73 eV and 1.05 eV, respectively were further obtained. In the PEC reduction of CO2 process, methanol and ethanol were two major products identified by chromatography. Their contents reached 1.00 mmol L(-1) cm(-2) and 107.38 μmol L(-1) cm(-2) after 6 h, respectively. This high-efficiency catalyst with photoelectric dual catalytic interfaces has a great guidance and reference significance for CO2 reduction to liquid carbon fuels. PMID:24121703

  13. Growth and characterization of electrodeposited Cu2O thin films

    NASA Astrophysics Data System (ADS)

    Laidoudi, S.; Bioud, A. Y.; Azizi, A.; Schmerber, G.; Bartringer, J.; Barre, S.; Dinia, A.

    2013-11-01

    This work demonstrates the electrodeposition of cuprous oxide (Cu2O) thin films onto a fluorine-doped tin oxide (FTO)-coated conducting glass substrates from Cu(II) sulfate solution with C6H8O7 chelating agent. During cyclic voltammetry experiences, the potential interval where the electrodeposition of Cu2O is carried out was established. The thin films were obtained potentiostatically and were characterized through different techniques. From the Mott-Schottky measurements, the flat-band potential and the acceptor density for the Cu2O thin films are determined. All the films showed a p-type semiconductor character with a carrier density varying between 2.41 × 1018 cm-3 and 5.38 × 1018 cm-3. This little difference is attributed to the increase of the stoichiometric defects in the films with the deposition potential. Atomic force microscopy analysis showed that the Cu2O thin films obtained at high potential are more homogenous in appearance and present lower crystallites size. X-ray diffraction measurements indicate a cubic structure with good crystallization state and the deposition potential was found to have an influence on the size of the crystallites. The optical measurements show a direct band gap between 2.07-2.49 eV depending on the applied potential.

  14. Electro-synthesis of Sn-Co nanowires in alumina membranes.

    PubMed

    Ferrara, G; Inguanta, R; Piazza, S; Sunseri, C

    2010-12-01

    A fabrication process of amorphous nanowires of Sn-Co alloys, based on electrodeposition into anodic alumina membranes, is described. It is shown that nanowires of tin-cobalt alloys with different compositions can be produced by varying electrodeposition time and concentration ratio of salts dissolved into the electrolytic bath. Importance of the chelating agent to produce amorphous Sn-Co alloys has also been addressed. Electrodepositions were carried out potentiostatically at -1 V versus Saturated Calomel Electrode and 60 degrees C for times ranging from 10 to 90 minutes; the atomic fraction of Co2+ in the aqueous electrolyte (Co2+/(Co2+ + Sn2+)) was varied from 0.33 to 0.67. Nanowires aspect ratio (height/width) was controlled by adjusting the deposition time. Alloys were characterized by scanning electron microscopy and X-ray diffraction; compositional analysis was performed by energy dispersive spectroscopy and induced coupled plasma. The highest concentration of Co in the alloy was found after 90 min of electrodeposition from a bath containing 67% of Co2+. PMID:21121335

  15. In situ electrochemical STM study of platinum nanodot arrays on highly oriented pyrolythic graphite prepared by electron beam lithography

    NASA Astrophysics Data System (ADS)

    Foelske-Schmitz, A.; Peitz, A.; Guzenko, V. A.; Weingarth, D.; Scherer, G. G.; Wokaun, A.; Kötz, R.

    2012-12-01

    Model electrodes consisting of platinum dots with a mean diameter of (30 ± 5) nm and heights of 3-5 nm upon highly oriented pyrolytic graphite (HOPG) were prepared by electron beam lithography and subsequent sputtering. The Pt nanodot arrays were stable during scanning tunnelling microscopy (STM) measurements in air and in sulphuric acid electrolyte, indicating the presence of "anchors", immobilising the dots on the HOPG surface. Electrochemical STM was used to visualise potential induced Pt, carbon and Pt-influenced carbon corrosion in situ in 0.5 M sulphuric acid under ambient conditions. Potentiostatic hold experiments show that the Pt dots start to disappear at electrode potentials of E > 1.4 V vs. SHE. With increasing time and potential a hole pattern congruent to the original dot pattern appears on the HOPG basal planes. Corrosion and peeling of the HOPG substrate could also be followed in situ. Dissolution of Pt dots appears to be accelerated for potential cycling experiments compared to the potential hold statistics.

  16. Electrochemical generation of oxygen. 1: The effects of anions and cations on hydrogen chemisorption and anodic oxide film formation on platinum electrode. 2: The effects of anions and cations on oxygen generation on platinum electrode

    NASA Technical Reports Server (NTRS)

    Huang, C. J.; Yeager, E.; Ogrady, W. E.

    1975-01-01

    The effects were studied of anions and cations on hydrogen chemisorption and anodic oxide film formation on Pt by linear sweep voltammetry, and on oxygen generation on Pt by potentiostatic overpotential measurement. The hydrogen chemisorption and anodic oxide film formation regions are greatly influenced by anion adsorption. In acids, the strongly bound hydrogen occurs at more cathodic potential when chloride and sulfate are present. Sulfate affects the initial phase of oxide film formation by produced fine structure while chloride retards the oxide-film formation. In alkaline solutions, both strongly and weakly bound hydrogen are influenced by iodide, cyanide, and barium and calcium cations. These ions also influence the oxide film formation. Factors considered to explain these effects are discussed. The Tafel slope for oxygen generation was found to be independent on the oxide thickness and the presence of cations or anions. The catalytic activity indicated by the exchange current density was observed decreasing with increasing oxide layer thickness, only a minor dependence on the addition of certain cations and anions was found.

  17. Integrated circuit-based electrochemical sensor for spatially resolved detection of redox-active metabolites in biofilms

    PubMed Central

    Bellin, Daniel L.; Sakhtah, Hassan; Rosenstein, Jacob K.; Levine, Peter M.; Thimot, Jordan; Emmett, Kevin; Dietrich, Lars E. P.; Shepard, Kenneth L.

    2014-01-01

    Despite advances in monitoring spatiotemporal expression patterns of genes and proteins with fluorescent probes, direct detection of metabolites and small molecules remains challenging. A technique for spatially resolved detection of small molecules would benefit the study of redox-active metabolites produced by microbial biofilms, which can drastically affect colony development. Here we present an integrated circuit-based electrochemical sensing platform featuring an array of working electrodes and parallel potentiostat channels. “Images” over a 3.25 × 0.9 mm area can be captured with a diffusion-limited spatial resolution of 750 μm. We demonstrate that square wave voltammetry can be used to detect, identify, and quantify (for concentrations as low as 2.6 μM) four distinct redox-active metabolites called phenazines. We characterize phenazine production in both wild-type and mutant Pseudomonas aeruginosa PA14 colony biofilms, and find correlations with fluorescent reporter imaging of phenazine biosynthetic gene expression. PMID:24510163

  18. Electrochemical Testing of Ni-Cr-Mo-Gd Alloys

    SciTech Connect

    T. E. Lister; R. E. Mizia; H. Tian

    2005-10-01

    The waste package site recommendation design specified a boron-containing stainless steel, Neutronit 976/978, for fabrication of the internal baskets that will be used as a corrosion-resistant neutron-absorbing material. Recent corrosion test results gave higher-than-expected corrosion rates for this material. The material callout for these components has been changed to a Ni-Cr-Mo-Gd alloy (ASTM-B 932-04, UNS N06464) that is being developed at the Idaho National Laboratory. This report discusses the results of initial corrosion testing of this material in simulated in-package environments that could contact the fuel baskets after breach of the waste package outer barrier. The corrosion test matrix was executed using the potentiodynamic and potentiostatic electrochemical test techniques. The alloy performance shows low rates of general corrosion after initial removal of a gadolinium-rich second phase that intersects the surface. The high halide-containing test solutions exhibited greater tendencies toward initiation of crevice corrosion.

  19. Analysis of gas products from direct utilization of carbon in a solid oxide fuel cell

    NASA Astrophysics Data System (ADS)

    Siengchum, Tritti; Guzman, Felipe; Chuang, Steven S. C.

    2012-09-01

    The evolution of gases from direct utilization of carbon in a solid oxide fuel cell (C-SOFC) was studied by potentiostatic/galvanostatic discharge of a fuel cell with coconut carbon, a carbonaceous material with low ash and sulfur content. Operation of C-SOFC at 750 °C produced less CO and more CO2 than those predicted by thermodynamic calculation using total Gibbs free energy minimization method. The addition of CO2 to the anode chamber increased CO formation and maximum power density from 0.09 W cm-2 to 0.13 W cm-2, indicating the occurrence of Boudouard reaction (CO2 + C ⇔ 2CO) coupling with CO electrochemical oxidation on the C-SOFC. Analysis of CO and CO2 concentration as a function of current and voltage revealed that electricity was mainly produced from the electrochemical oxidation of carbon at low current density and produced from the electrochemical oxidation of CO at high current density. The results suggest the electrochemical oxidation of solid carbon is more mass transfer limited than electrochemical oxidation of CO.

  20. Submicron patterned metal hole etching

    DOEpatents

    McCarthy, Anthony M.; Contolini, Robert J.; Liberman, Vladimir; Morse, Jeffrey

    2000-01-01

    A wet chemical process for etching submicron patterned holes in thin metal layers using electrochemical etching with the aid of a wetting agent. In this process, the processed wafer to be etched is immersed in a wetting agent, such as methanol, for a few seconds prior to inserting the processed wafer into an electrochemical etching setup, with the wafer maintained horizontal during transfer to maintain a film of methanol covering the patterned areas. The electrochemical etching setup includes a tube which seals the edges of the wafer preventing loss of the methanol. An electrolyte composed of 4:1 water: sulfuric is poured into the tube and the electrolyte replaces the wetting agent in the patterned holes. A working electrode is attached to a metal layer of the wafer, with reference and counter electrodes inserted in the electrolyte with all electrodes connected to a potentiostat. A single pulse on the counter electrode, such as a 100 ms pulse at +10.2 volts, is used to excite the electrochemical circuit and perform the etch. The process produces uniform etching of the patterned holes in the metal layers, such as chromium and molybdenum of the wafer without adversely effecting the patterned mask.

  1. Polyphenol biosensor based on laccase immobilized onto silver nanoparticles/multiwalled carbon nanotube/polyaniline gold electrode.

    PubMed

    Rawal, Rachna; Chawla, Sheetal; Pundir, C S

    2011-12-15

    Laccase purified from Ganoderma sp. was immobilized covalently onto electrochemically deposited silver nanoparticles (AgNPs)/carboxylated multiwalled carbon nanotubes (cMWCNT)/polyaniline (PANI) layer on the surface of gold (Au) electrode. A polyphenol biosensor was fabricated using this enzyme electrode (laccase/AgNPs/cMWCNT/PANI/Au electrode) as the working electrode, Ag/AgCl as the reference electrode, and platinum (Pt) wire as the auxiliary electrode connected through a potentiostat. The biosensor showed optimal response at pH 5.5 (0.1 M acetate buffer) and 35°C when operated at a scan rate of 50 mV s(-1). Linear range, response time, and detection limit were 0.1-500 μM, 6 s, and 0.1 μM, respectively. The sensor was employed for the determination of total phenolic content in tea, alcoholic beverages, and pharmaceutical formulations. The enzyme electrode was used 200 times over a period of 4 months when stored at 4°C. The biosensor has an advantage over earlier enzyme sensors in that it has no leakage of enzyme during reuse and is unaffected by the external environment due to the protective PANI microenvironment. PMID:21855525

  2. Corrosion inhibition of a mild steel by aniline and alkylamines in acidic solutions

    SciTech Connect

    Luo, H.; Han, K.N.; Guan, Y.C.

    1998-09-01

    Corrosion inhibition of a mild steel in acid solutions by alkylamines (ALK-AM) and aniline hydrochloric (ANL-HCl) salts was investigated in the presence of sodium sulfate (Na{sub 2}SO{sub 4}) and sodium chloride (NaCl) using a potentiostat, a contact-angle goniometer, a scanning electron microscope (SEM), a Fourier transform infrared spectrometer (FTIR), and an atomic force microscope (AFM). Results showed chloride ions (Cl{sup {minus}}) had a pronounced effect on inhibition of amines and ANL for corrosion of mild steel. In the presence of Cl{sup {minus}} ions, cationic types of surfactants (ALK-AM and ANL) were attached to the surface through formation of chloride precipitate at the surface. In the absence of the organic inhibitors, corrosion initiated along grain boundaries of ferrite and pearlite structures. In the presence of the organic inhibitor, however, the steel surface was covered by an organic salt precipitation, and the corrosion rate was reduced significantly.

  3. Corrosion inhibition of copper with benzotriazole and other organic surfactants

    SciTech Connect

    Ling, Y.; Guan, Y.; Han, K.N.

    1995-05-01

    The corrosion behavior of copper with various organic inhibitors in aerated solutions at pH 1 to pH 2 was studied using a potentiostat. The inhibitors studied included benzotriazole (BTAH), hydroxy benzophenoximes, L-hydroxy-5-nonylacetophenone oxime, and sodium octyl hydroxamate (SOH). BTAH was shown to be the most effective of the inhibitors tested. Morphology of the copper substrate after corrosion in the presence and absence of BTAH was examined using scanning electron microscopy (SEM). Fourier transform infrared spectroscopy (FTIR) was used to identify the spectra of the adsorbed complexes (BTA). The surface film was identified as a polymeric Cu(I)-BTA complex that totally covered the copper surface, exhibiting strong corrosion inhibition. The formation of Cu(I)-BTA was found to have been accomplished after the adsorption of BTAH on the copper surface. The effect of annealing of copper plate on the rate of corrosion also was investigated, and results indicated that the annealed copper exhibited better corrosion resistance than copper plate that had not been annealed.

  4. Strong Photo-Amplification Effects in Flexible Organic Capacitors with Small Molecular Solid-State Electrolyte Layers Sandwiched between Photo-Sensitive Conjugated Polymer Nanolayers.

    PubMed

    Lee, Hyena; Kim, Jungnam; Kim, Hwajeong; Kim, Youngkyoo

    2016-01-01

    We demonstrate strong photo-amplification effects in flexible organic capacitors which consist of small molecular solid-state electrolyte layers sandwiched between light-sensitive conjugated polymer nanolayers. The small molecular electrolyte layers were prepared from aqueous solutions of tris(8-hydroxyquinoline-5-sulfonic acid) aluminum (ALQSA3), while poly(3-hexylthiophene) (P3HT) was employed as the light-sensitive polymer nanolayer that is spin-coated on the indium-tin oxide (ITO)-coated poly(ethylene terephthalate) (PET) film substrates. The resulting capacitors feature a multilayer device structure of PET/ITO/P3HT/ALQSA3/P3HT/ITO/PET, which were mechanically robust due to good adhesion between the ALQSA3 layers and the P3HT nanolayers. Results showed that the specific capacitance was increased by ca. 3-fold when a white light was illuminated to the flexible organic multilayer capacitors. In particular, the capacity of charge storage was remarkably (ca. 250-fold) enhanced by a white light illumination in the potentiostatic charge/discharge operation, and the photo-amplification functions were well maintained even after bending for 300 times at a bending angle of 180(o). PMID:26846891

  5. Electrochemical Polishing Applications and EIS of a Vitamin B{sub 4}-Based Ionic Liquid

    SciTech Connect

    Wixtrom, Alex I.; Buhler, Jessica E.; Reece, Charles E.; Abdel-Fattah, Tarek M.

    2013-01-01

    Modern particle accelerators require minimal interior surface roughness for Niobium superconducting radio frequency (SRF) cavities. Polishing of the Nb is currently achieved via electrochemical polishing with concentrated mixtures of sulfuric and hydrofluoric acids. This acid-based approach is effective at reducing the surface roughness to acceptable levels for SRF use, but due to acid-related hazards and extra costs (including safe disposal of used polishing solutions), an acid-free method would be preferable. This study focuses on an alternative electrochemical polishing method for Nb, using a novel ionic liquid solution containing choline chloride, also known as Vitamin B{sub 4} (VB{sub 4}). Potentiostatic electrochemical impedance spectroscopy (EIS) was also performed on the VB4-based system. Nb polished using the VB4-based method was found to have a final surface roughness comparable to that achieved via the acid-based method, as assessed by atomic force microscopy (AFM). These findings indicate that acid-free VB{sub 4}-based electrochemical polishing of Nb represents a promising replacement for acid-based methods of SRF cavity preparation.

  6. Improvement in direct methanol fuel cell performance by treating the anode at high anodic potential

    NASA Astrophysics Data System (ADS)

    Joghee, Prabhuram; Pylypenko, Svitlana; Wood, Kevin; Corpuz, April; Bender, Guido; Dinh, Huyen N.; O'Hayre, Ryan

    2014-01-01

    This work investigates the effect of a high anodic potential treatment protocol on the performance of a direct methanol fuel cell (DMFC). DMFC membrane electrode assemblies (MEAs) with PtRu/C (Hi-spec 5000) anode catalyst are subjected to anodic treatment (AT) at 0.8 V vs. DHE using potentiostatic method. Despite causing a slight decrease in the electrochemical surface area (ECSA) of the anode, associated with ruthenium dissolution, AT results in significant improvement in DMFC performance in the ohmic and mass transfer regions and increases the maximum power density by 15%. Furthermore, AT improves the long-term DMFC stability by reducing the degradation of the anode catalyst. From XPS investigation, it is hypothesized that the improved performance of AT-treated MEAs is related to an improved interface between the catalyst and Nafion ionomer. Among potential explanations, this improvement may be caused by incorporation of the ionomer within the secondary pores of PtRu/C agglomerates, which generates a percolating network of ionomer between PtRu/C agglomerates in the catalyst layer. Furthermore, the decreased concentration of hydrophobic CF2 groups may help to enhance the hydrophilicity of the catalyst layer, thereby increasing the accessibility of methanol and resulting in better performance in the high current density region.

  7. Kinetics and mechanism of the electrochemical formation of iron oxidation products on steel immersed in sour acid media.

    PubMed

    Hernndez-Espejel, Antonio; Palomar-Pardav, Manuel; Cabrera-Sierra, Romn; Romero-Romo, Mario; Ramrez-Silva, Mara Teresa; Arce-Estrada, Elsa M

    2011-03-01

    From electrochemical techniques (cyclic voltammetry, potential steps, and EIS), XRD, and SEM-EDX, the kinetics and mechanism of anodic film formation applying anodic potential steps on steel immersed in sour acid media was determined. It was found, from a thermodynamic analysis, based on equilibrium phase diagrams of the system considered in this work, that iron oxidation may produce different new solid phases, depending on the applied potential, the first being the iron oxidation associated with formation of FeS((c)) species, which in turn can be reoxidized to FeS(2(c)) or even to Fe(2)O(3(c)) at higher potential values. From analysis of the corresponding experimental potentiostatic current density transients, it was concluded that the electrochemical anodic film formation involves an E(1)CE(2) mechanism, whereby the first of the two simultaneous processes were the Fe electrochemical oxidation (E(1)) followed by FeS precipitation (C) that occurs by 3D nucleation and growth limited by mass transfer reaction and FeS oxidation (E(2)) forming a mix of different stoichiometry iron sulphides and oxides. From EIS measurements, it was revealed that the anodic film's charge transfer resistance diminishes as the potential applied for its formation becomes more anodic, thus behaving poorly against corrosion. PMID:21302956

  8. Stretchable, multiplexed pH sensors with demonstrations on rabbit and human hearts undergoing ischemia.

    PubMed

    Chung, Hyun-Joong; Sulkin, Matthew S; Kim, Jong-Seon; Goudeseune, Camille; Chao, Hsin-Yun; Song, Joseph W; Yang, Sang Yoon; Hsu, Yung-Yu; Ghaffari, Roozbeh; Efimov, Igor R; Rogers, John A

    2014-01-01

    Stable pH is an established biomarker of health, relevant to all tissues of the body, including the heart. Clinical monitoring of pH in a practical manner, with high spatiotemporal resolution, is particularly difficult in organs such as the heart due to its soft mechanics, curvilinear geometry, heterogeneous surfaces, and continuous, complex rhythmic motion. The results presented here illustrate that advanced strategies in materials assembly and electrochemical growth can yield interconnected arrays of miniaturized IrOx pH sensors encapsulated in thin, low-modulus elastomers to yield conformal monitoring systems capable of noninvasive measurements on the surface of the beating heart. A thirty channel custom data acquisition system enables spatiotemporal pH mapping with a single potentiostat. In vitro testing reveals super-Nernstian sensitivity with excellent uniformity (69.9 ± 2.2 mV/pH), linear response to temperature (-1.6 mV °C(-1) ), and minimal influence of extracellular ions (<3.5 mV). Device examples include sensor arrays on balloon catheters and on skin-like stretchable membranes. Real-time measurement of pH on the surfaces of explanted rabbit hearts and a donated human heart during protocols of ischemia-reperfusion illustrate some of the capabilities. Envisioned applications range from devices for biological research, to surgical tools and long-term implants. PMID:23868871

  9. Electrochemical deposition and microstructural characterization of AlCrFeMnNi and AlCrCuFeMnNi high entropy alloy thin films

    NASA Astrophysics Data System (ADS)

    Soare, V.; Burada, M.; Constantin, I.; Mitrică, D.; Bădiliţă, V.; Caragea, A.; Târcolea, M.

    2015-12-01

    Al-Cr-Fe-Mn-Ni and Al-Cr-Cu-Fe-Mn-Ni high entropy alloy thin films were prepared by potentiostatic electrodeposition and the microstructure of the deposits was investigated. The thin films were co-deposited in an electrolyte based on a DMF (N,N-dimethylformamide)-CH3CN (acetonitrile) organic compound. The energy dispersive spectrometry investigation (EDS) indicated that all the five respectively six elements were successfully co-deposited. The scanning electron microscopy (SEM) analysis revealed that the film consists of compact and uniform particles with particle sizes of 500 nm to 4 μm. The X-ray diffractometry (XRD) patterns indicated that the as-deposited thin films were amorphous. Body-centered-cubic (BCC) structures were identified by XRD after the films were annealed at various temperatures under inert Ar atmosphere. The alloys adhesion on the substrate was determined by the scratch-testing method, with higher values obtained for the Al-Cr-Cu-Fe-Mn-Ni alloy.

  10. Electrodeposited ZnO films with high UV emission properties

    SciTech Connect

    Matei, Elena; Enculescu, Ionut

    2011-11-15

    Highlights: {yields} Electrodeposition of ZnO from nitrate baths is investigated. {yields} The influence of process parameters on morphological and optical properties is studied. {yields} Experimental conditions to fabricate ZnO films with high UV emission were found. -- Abstract: We report here our results in the preparation of ZnO films with high UV band to band characteristic luminescence emission by potentiostatic electrodeposition. Zinc nitrate aqueous baths with different concentration and additives were employed for the preparation of the films on platinum substrates. We focused our research in determining how the electrodeposition bath composition, i.e. zinc nitrate concentration and addition of KCl or polyvinyl pyrolidone and applied overpotential influence the morphological and optical properties of the oxide films. Scanning electron microscopy was employed for characterizing the films in terms of morphology. Optical reflection, photoluminescence spectroscopy and cathodoluminescence were used for determining the optical characteristics of the samples. The morphology of the deposit varies from hexagonal prisms to platelets as a function of the deposition rate. This experimental parameter also influences the luminescence properties. We found that at low deposition rates high UV luminescent material is obtained.

  11. New secondary batteries utilizing electronically conductive polypyrrole cathode

    NASA Astrophysics Data System (ADS)

    Yeu, Taewhan

    1991-05-01

    To gain a better understanding of the dynamic behavior in electronically conducting polypyrroles and to provide guidance toward designs of new secondary batteries based on these polymers, two mathematical models are developed; one for the potentiostatically controlled switching behavior of polypyrrole film, and one for the galvanostatically controlled charge/discharge behavior of lithium/polypyrrole secondary battery cell. The first model is used to predict the profiles of electrolyte concentrations, charge states, and electrochemical potentials within the thin polypyrrole film during switching process as functions of applied potential and position. Thus, the detailed mechanisms of charge transport and electrochemical reaction can be understood. Sensitivity analysis is performed for independent parameters, describing the physical and electrochemical characteristic of polypyrrole film, to verify their influences on the model performance. The values of independent parameters are estimated by comparing model predictions with experimental data obtained from identical conditions. The second model is used to predict the profiles of electrolyte concentrations, charge state, and electrochemical potentials within the battery system during charge and discharge processes as functions of time and position. Energy and power densities are estimated from model predictions and compared with existing battery systems. The independent design criteria on the charge and discharge performance of the cell are provided by studying the effects of design parameters.

  12. A 1000-cell SOFC reactor for domestic cogeneration

    NASA Astrophysics Data System (ADS)

    Alston, T.; Kendall, K.; Palin, M.; Prica, M.; Windibank, P.

    A cogeneration system was built using 1000 cells with the intention of supplying 30 kW of hot water and 500 W of power. The basis of the cogenerator was the small tubular SOFC design. 8Y zirconia was mixed into a plastic paste and extruded to form thin-walled tubes. The process produced a zirconia material with high strength and good electrical properties. After drying and firing to full density, electrodes were coated onto the inner and outer surfaces of the electrolyte, then sintered. Current collecting wires were wound around the tubular cells and the tubes were assembled into a reactor. Either hydrogen or a premix of natural gas and air was fed through the tubes and ignited by a hot wire. The ignition shock did not damage the cells in any way. Cycling was achieved within minutes. A steel heat exchanger/recuperator was used to feed hot air to the cell stack. The electrical output was measured via a potentiostat.

  13. Effect of Acidified Feronia elephantum Leaf Extract on the Corrosion Behavior of Mild Steel

    NASA Astrophysics Data System (ADS)

    Muthukrishnan, Pitchaipillai; Prakash, Periakaruppan; Ilayaraja, Murugan; Jeyaprabha, Balasubramanian; Shankar, Karikalan

    2015-03-01

    Mild steel is used as a structural material for pipes, tank, reaction vessels, etc. which are known to corrode invariably in contact with various solvents. From the view point of a nation's economy and financial implications of corrosion hazard, it is necessary to adopt appropriate means and ways to reduce the losses due to corrosion. The use of eco-friendly corrosion inhibitors are increasing day by day. Feronia elephantum leaf extract (FELE) has been tested as eco-friendly corrosion inhibitor for A262 mild steel in 1 M H2SO4 and 1 M HCl solutions using non-electrochemical (Gravimetric, X-ray diffraction analysis, scanning electron microscopy, and Fourier transform infrared spectroscopy) and electrochemical techniques (open circuit potential, potentiostatic polarization, and electrochemical impedance measurements). The protection efficiency is found to increase with increase in FELE concentration but decrease with temperature, which is suggestive of physical adsorption mechanism. The adsorption of FELE on mild steel surface obeys the Langmuir adsorption isotherm. SEM results confirm the formation of a protective layer by FELE over mild steel surface.

  14. Electrodeposition of Cu-Pd alloys onto electrophoretic deposited carbon nanotubes for nitrate electroreduction

    NASA Astrophysics Data System (ADS)

    Zhang, Qiu; Ding, Liang; Cui, Hao; Zhai, Jianping; Wei, Zhongbo; Li, Qin

    2014-07-01

    Copper-palladium (Cu-Pd) alloys have been electrodeposited onto carbon nanotubes, which were uniformly and stably deposited on Ti plates via electrophoretic deposition. Electrodes with a wide range of Cu/Pd atomic ratios were fabricated by potentiostatic coelectrodeposition of Cu and Pd onto Ti/CNTs. They were characterized by energy-dispersive X-ray analyzer, X-ray diffraction and tested for nitrate electroreduction. The electrode deposited in bath with 5 mM Cu2+ and 5 mM Pd2+ (Ti/CNTs/Cu5-Pd5) possessed outstanding stability as well as the highest electrocatalytic activity with the best nitrate conversion yield and proper N2 selectivity, indicating a synergistic effect of Cu and Pd. X-ray photoelectron spectroscopy and scanning electron microscopy analysis of Ti/CNTs/Cu5-Pd5 and Ti/Cu5-Pd5 revealed that CNTs played a remarkable role in the homogeneous formation of the bimetal, significantly improving the alloy's electrocatalytic activity and stability. The fabricated Ti/CNTs/Cu5-Pd5 was proved to be a promising electrode for nitrate electroreduction.

  15. Synthesis of single-walled carbon nanotubes and graphene composite in arc for ultracapacitors

    NASA Astrophysics Data System (ADS)

    Li, Jian; Cheng, Xiaoqian; Shashurin, Alexey; Keidar, Michael

    2012-10-01

    Arc discharge supported by the erosion of graphite anode is considered as one of the most practical and efficient methods to synthesize various carbon nanostructures such as single-walled carbon nanotubes (SWCNT) and graphene with minimal defects and large yield due to the relatively high synthesis temperature and eco-friendly growth mechanism. By introducing a non-uniform magnetic field during synthesis process, large-scale graphene and high-purity SWCNT can be obtained in one step. In addition, the yield of graphene can be controlled by external parameters, such as the type and pressure of buffer gas, the temperature of substrate, and so on. Possessing the properties of highly accessible surface area and good electrical conductivity, the composite of graphene and SWCNT are promising nanomaterials for the electrodes of ultracapacitor, which can store electric energy with high level of capacitance. In this work, we fabricated electrodes of ultracapacitor based on nanostructures composite by wire-wound rod coating method, characterized them by SEM, EDX and Raman spectroscopy, and tested the performance by a potentiostat/galvanostat.

  16. Evaluation of a diffusion/trapping model for hydrogen ingress in high-strength alloys. Final technical report, November 1988-November 1990

    SciTech Connect

    Pound, B.G.

    1990-11-14

    The objective of this research was to obtain the hydrogen ingress and trapping characteristics for a range of microstructures and so identify the dominant type of irreversible trap in different alloys. A diffusion/trapping model was used in conjunction with a potentiostatic pulse technique to study the ingress of hydrogen in three precipitation-hardened alloys (Inconel 718, Incoloy 925, and 18Ni maraging steel), two work-hardened alloys (Inconel 625 and Hastelloy C-276), titanium (pure and grade 2), and copper-enriched AISI 4340 steel in 1 mol/L acetic acid-1 mol/L sodium acetate containing 15 ppm arsenic oxide. In all cases except pure titanium, the data were shown to fit the interface-control form of the model and values were determined for the irreversible trapping constants (k) and the flux of hydrogen into the alloys. The density of irreversible trap defects were calculated from k and generally found to be in close agreement with the concentration of a specific heterogeneity in each alloy. Moreover, the trapping constants for the alloys were found to be consistent with their relative susceptibilities to hydrogen embrittlement.

  17. Electrodeposition of Nanocrystalline Chromium Coatings Based on 1-Butyl-3-Methylimidazolium-Bromide Ionic Liquid.

    PubMed

    He, Xinkuai; Zhu, Qingyun; Hou, Bailong; Cai, Youxing; Li, Chen; Fu, Liqin; Wu, Luye

    2015-12-01

    The electrochemical behavior of trivalent chromium reduction from 1-butyl-3-methylimidazolium-bromide ([BMIM]Br) ionic liquid is studied. The result of cyclic voltammetry shows that the Cr(III) reduction is irreversible and occurs in two steps, Cr(III)to Cr(II), and Cr(II) to Cr(0), respectively. In the electrochemical impedance spectroscopy measurements, the preferable equivalent circuit is made to fit the experimental data. The effects of electroplating parameters on coating thickness and electrodepositon rate are investigated by potentiostatic method on Cu electrode from Cr(III)-[BMIM]Br solution. The results show that the temperature and depositing potential have great effect on the coating thickness and electrodeposition rate. The surface morphology and composition of deposited Cr are investigated using scanning electron microscope (SEM) and energy-dispersive spectroscopy (EDS). SEM analysis shows that chromium electrodeposits obtained on Cu electrodes present a ball-like structure. EDS analysis shows that the coatings are composed of Cr. Moreover, the corrosion resistance of the as-deposited chromium layer is evaluated using polarization curves. The results show that the corrosion resistance of the chromium coatings obtained at higher potential is better. PMID:26682363

  18. SEM method for direct visual tracking of nanoscale morphological changes of platinum based electrocatalysts on fixed locations upon electrochemical or thermal treatments.

    PubMed

    Zorko, Milena; Jozinovi?, Barbara; Bele, Marjan; Hodnik, Nejc; Gaber?ek, Miran

    2014-05-01

    A general method for tracking morphological surface changes on a nanometer scale with scanning electron microscopy (SEM) is introduced. We exemplify the usefulness of the method by showing consecutive SEM images of an identical location before and after the electrochemical and thermal treatments of platinum-based nanoparticles deposited on a high surface area carbon. Observations reveal an insight into platinum based catalyst degradation occurring during potential cycling treatment. The presence of chloride clearly increases the rate of degradation. At these conditions the dominant degradation mechanism seems to be the platinum dissolution with some subsequent redeposition on the top of the catalyst film. By contrast, at the temperature of 60C, under potentiostatic conditions some carbon corrosion and particle aggregation was observed. Temperature treatment simulating the annealing step of the synthesis reveals sintering of small platinum based composite aggregates into uniform spherical particles. The method provides a direct proof of induced surface phenomena occurring on a chosen location without the usual statistical uncertainty in usual, random SEM observations across relatively large surface areas. PMID:24662366

  19. Corrosion inhibitor storage and release property of TiO{sub 2} nanotube powder synthesized by rapid breakdown anodization method

    SciTech Connect

    Arunchandran, C.; Ramya, S.; George, R.P.; Kamachi Mudali, U.

    2013-02-15

    Graphical abstract: Display Omitted Highlights: ► TiO{sub 2} nanotube powders were synthesized by rapid breakdown anodization method. ► Benzotriazole was loaded into the TiO{sub 2} nanotube powders. ► Low pH induced release of benzotriazole from TiO{sub 2} nanotube powders was proved. -- Abstract: Titanium dioxide (TiO{sub 2}) is one of the most studied substances in material science due to its versatile properties and diverse applications. In this study titanium dioxide nanotube powder were synthesized by rapid breakdown anodization (RBA) method. The synthesis involved potentiostatic anodization of titanium foil in 0.1 M HClO{sub 4} electrolyte under an applied voltage of 20 V and rapid stirring. The morphology and the phase of titanium dioxide nanotube powder were studied using field emission scanning electron microscopy, laser Raman spectroscopy and high resolution transmission electron microscopy. Benzotriazole was chosen as model inhibitor to evaluate TiO{sub 2} nanotube powder's corrosion inhibitor loading and releasing properties. The storage and release properties of TiO{sub 2} nanotube powder were studied using UV–visible spectroscopy and thermogravimetric analysis.

  20. Electrochemical removal of hydrogen atoms in Mg-doped GaN epitaxial layers

    SciTech Connect

    Lee, June Key E-mail: hskim7@jbnu.ac.kr; Hyeon, Gil Yong; Tawfik, Wael Z.; Choi, Hee Seok; Ryu, Sang-Wan; Jeong, Tak; Jung, Eunjin; Kim, Hyunsoo E-mail: hskim7@jbnu.ac.kr

    2015-05-14

    Hydrogen atoms inside of an Mg-doped GaN epitaxial layer were effectively removed by the electrochemical potentiostatic activation (EPA) method. The role of hydrogen was investigated in terms of the device performance of light-emitting diodes (LEDs). The effect of the main process parameters for EPA such as solution type, voltage, and time was studied and optimized for application to LED fabrication. In optimized conditions, the light output of 385-nm LEDs was improved by about 26% at 30 mA, which was caused by the reduction of the hydrogen concentration by ∼35%. Further removal of hydrogen seems to be involved in the breaking of Ga-H bonds that passivate the nitrogen vacancies. An EPA process with high voltage breaks not only Mg-H bonds that generate hole carriers but also Ga-H bonds that generate electron carriers, thus causing compensation that impedes the practical increase of hole concentration, regardless of the drastic removal of hydrogen atoms. A decrease in hydrogen concentration affects the current-voltage characteristics, reducing the reverse current by about one order and altering the forward current behavior in the low voltage region.

  1. Electrochemical glucose oxidation on dendritic cuprous oxide film fabricated by PSS-assisted electrochemical deposition

    NASA Astrophysics Data System (ADS)

    Yang, Ming; Jin, Xiaoqi; Huang, Qiao

    2011-02-01

    Cuprous oxides (Cu 2O) with different morphologies were deposited on F-doped tin oxide (FTO) covered glass substrates by potentiostatic deposition. The as-deposited samples were characterized by XRD, BET surface area and SEM. The effects of Poly(styrene sulfonic acid) sodium salt (PSS) on the crystal morphologies of Cu 2O were studied. Different crystal morphologies of Cu 2O can be obtained by varying the concentrations of PSS in the electrolytes. The formation of dendritic microstructure in Cu 2O film depends on the concentration of PSS in the electrolyte. Dendritic Cu 2O crystals formed gradually with the increase of the concentration of PSS in the electrolyte from 0 to 4 g L -1. More symmetrical Cu 2O crystals appear when the concentration of PSS is changed from 4 to 8 g L -1. However, the Cu 2O nanoparticles formed instead of dendritic Cu 2O crystals if the concentration of PSS reaches to 12 g L -1, which is due to the slower diffusion rate of reactive species in high concentration of PSS. The as-deposited Cu 2O thin films with different morphologies all exhibit the electrochemical glucose oxidation properties. The improved performance of glucose oxidation is achieved on the dendritic Cu 2O film electrode. The result indicates that the dendritic microstructure is beneficial for decreasing the resistance and improving transportation and diffusion of reactants and products.

  2. Short-term canine implantation of a glucose monitoring-telemetry device.

    PubMed

    Atanasov, P; Yang, S; Salehi, C; Ghindilis, A L; Wilkins, E

    1996-12-01

    In this study we report the development and short-term in vivo evaluation of an integrated implantable device consisting of an amperometric glucose biosensor, a miniature potentiostat, a FM signal transmitter, and power supply. The device (dimensions: 5.0 x 7.0 x 1.5 cm) was implanted under the skin of medium-size anaesthetized dog. The experimental set-up included several methods for data collection: analog recording via wired X-T chart recorders; data collection by wearable microprocessor--data logger, and remote data collection via antenna and receiver linked to a computer-based data acquisition system. The device (sensor) performance was evaluated in vitro prior to implantation, using different model solutions simulating the physiological environment. A linear response to glucose concentration was obtained up to 25 mM glucose, with a sensitivity of 0.5 microA/mM. The results of short-term subcutaneous implantation of the integrated device reveal adequate monitoring of an artificially-induced glycaemia. The delay-time was 3-7 minutes. These tests demonstrate the feasibility of data transmission by the telemetry system through the skin of a medium-sized dog and allow the commencement of chronic in vivo experimentation. PMID:8953555

  3. Strong Photo-Amplification Effects in Flexible Organic Capacitors with Small Molecular Solid-State Electrolyte Layers Sandwiched between Photo-Sensitive Conjugated Polymer Nanolayers

    PubMed Central

    Lee, Hyena; Kim, Jungnam; Kim, Hwajeong; Kim, Youngkyoo

    2016-01-01

    We demonstrate strong photo-amplification effects in flexible organic capacitors which consist of small molecular solid-state electrolyte layers sandwiched between light-sensitive conjugated polymer nanolayers. The small molecular electrolyte layers were prepared from aqueous solutions of tris(8-hydroxyquinoline-5-sulfonic acid) aluminum (ALQSA3), while poly(3-hexylthiophene) (P3HT) was employed as the light-sensitive polymer nanolayer that is spin-coated on the indium-tin oxide (ITO)-coated poly(ethylene terephthalate) (PET) film substrates. The resulting capacitors feature a multilayer device structure of PET/ITO/P3HT/ALQSA3/P3HT/ITO/PET, which were mechanically robust due to good adhesion between the ALQSA3 layers and the P3HT nanolayers. Results showed that the specific capacitance was increased by ca. 3-fold when a white light was illuminated to the flexible organic multilayer capacitors. In particular, the capacity of charge storage was remarkably (ca. 250-fold) enhanced by a white light illumination in the potentiostatic charge/discharge operation, and the photo-amplification functions were well maintained even after bending for 300 times at a bending angle of 180o. PMID:26846891

  4. UV/Vis/NIR Spectroelectrochemistry

    NASA Astrophysics Data System (ADS)

    Neudeck, Andreas; Marken, Frank; Compton, Richard G.

    Voltammetric techniques used in electrochemistry monitor the flow of current as a function of potential, time, and mass transport. A huge variety of different experiments are possible, giving information about reaction energies, reaction intermediates, and the kinetics of a process [1-4]. However, additional data are often required and are accessible, in particular, via in situ spectroelectrochemical approaches. By coupling a spectroscopic technique such as UV/Vis/NIR spectroscopy [5, 6] to an electrochemical experiment, a wealth of complementary information as a function of the potential, time, and mass transport is available. In a recently published book dedicated to spectroelectrochemical techniques [7] the diversity of methods and new chemical information obtained is apparent. Both spectroscopic information about short-lived unstable intermediates and spectroscopic information disentangling the composition of complex mixtures of reactants can be obtained. Figure II.6.1 shows a schematic diagram for the case of a computer-controlled potentiostat system connected to a conventional electrochemical cell (working electrode WE, reference electrode RE, counter electrode CE) and simultaneously controlling the emitter and detector of a spectrometer. This kind of experimental arrangement allows the electrochemical and the spectroscopic data to be recorded simultaneously and, therefore, in contrast to the analysis of two independent data sets, direct correlation of data as a function of time and potential is possible.

  5. Lab-on-a-bird: biophysical monitoring of flying birds.

    PubMed

    Gumus, Abdurrahman; Lee, Seoho; Ahsan, Syed S; Karlsson, Kolbeinn; Gabrielson, Richard; Guglielmo, Christopher G; Winkler, David W; Erickson, David

    2015-01-01

    The metabolism of birds is finely tuned to their activities and environments, and thus research on avian systems can play an important role in understanding organismal responses to environmental changes. At present, however, the physiological monitoring of bird metabolism is limited by the inability to take real-time measurements of key metabolites during flight. In this study, we present an implantable biosensor system that can be used for continuous monitoring of uric acid levels of birds during various activities including flight. The system consists of a needle-type enzymatic biosensor for the amperometric detection of uric acid in interstitial fluids. A lightweight two-electrode potentiostat system drives the biosensor, reads the corresponding output current and wirelessly transfers the data or records to flash memory. We show how the device can be used to monitor, in real time, the effects of short-term flight and rest cycles on the uric acid levels of pigeons. In addition, we demonstrate that our device has the ability to measure uric acid level increase in homing pigeons while they fly freely. Successful application of the sensor in migratory birds could open up a new way of studying birds in flight which would lead to a better understanding of the ecology and biology of avian movements. PMID:25880904

  6. Amperometric choline biosensor based on multiwalled carbon nanotubes/zirconium oxide nanoparticles electrodeposited on glassy carbon electrode.

    PubMed

    Pundir, S; Chauhan, N; Narang, J; Pundir, C S

    2012-08-01

    A bienzymatic choline biosensor was constructed by coimmobilizing acetylcholinesterase (AChE) and choline oxidase (ChO) onto nanocomposite of carboxylated multiwalled carbon nanotubes (c-MWCNTs) and zirconium oxide nanoparticles (ZrO(2)NPs) electrodeposited on the surface of a glassy carbon electrode (GCE) and using it (AChE-ChO/c-MWCNT/ZrO(2)NPs/GCE) as working electrode, Ag/AgCl as reference electrode, and Pt wire as auxiliary electrode connected through a potentiostat. The enzyme electrode was characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, and cyclic voltammetry (CV) studies, optimized, and evaluated. The biosensor exhibited optimum response within 4 s at +0.2V, pH 7.4, and 25 °C. The detection limit and working range of the biosensor were 0.01 μM and 0.05 to 200 μM, respectively. The half-life of the enzyme electrode was 60 days at 4 °C. The serum choline level, as measured by the biosensor, was 9.0 to 12.8 μmol/L (with a mean of 10.81 μmol/L) in apparently healthy persons and 5.0 to 8.4 μmol/L (with a mean of 6.53 μmol/L) in persons suffering from Alzheimer's disease. The enzyme electrode was unaffected by a number of serum substances. PMID:22561918

  7. Selective functionalization of gold arms of a surface plasmon polariton Mach-Zehnder interferometer for biosensing

    NASA Astrophysics Data System (ADS)

    Tencer, Michal; Berini, Pierre

    2009-06-01

    In long range surface plasmon polariton (LRSPP) sensing, in a Mach-Zehnder interferometer (MZI) configuration, gold arms have to respond differently to the analyte as to form layers with different refractive indices. This can be achieved if the arms are coated with different thiol-based self-assembled monolayers (SAMs), one of which should block adsorption and the other should specifically adsorb the analyte of interest. Since the MZI arms' width and the distance between them are in the micron range, such a chemical differentiation is a challenging task which nevertheless could be achieved with two techniques (1) Microspotting trough droplet confinement and manipulation using a solvophilic guide and (2) Toposelective electrochemical desorption of SAMs where the arms are subjected to different potentials. We found the latter approach the most promising because of its scalability to the wafer level. During the electrochemical desorption the potentials of both arms have to be independently controlled with a multi-channel potentiostat. Subsequent deposition of another SAM on the freed MZI arm is accomplished with minimal thiol exchange. The resulting MZI was analyzed and imaged by time-of-flight secondary ion mass spectrometry (ToF- SIMS) and with phase shift atomic force microscopy which confirms the desired MZI structure in which only one arm has specific affinity to one protein while the other would block any interaction.

  8. Carbon nanotube enhanced mediator-type biosensor for real-time monitoring of glucose concentrations in fish.

    PubMed

    Takase, Mai; Yoneyama, Yohei; Murata, Masataka; Hibi, Kyoko; Ren, Huifeng; Endo, Hideaki

    2012-05-01

    We have developed a mediator-type biosensor to rapidly monitor blood glucose concentrations in fish, which are an indicator of stress. Glucose oxidase was used to detect glucose concentrations and ferrocene was used to limit the effect of oxygen. We also improved the sensitivity and durability of the sensor for better performance. Single-walled carbon nanotubes were used to enhance sensor sensitivity. Affixing the carbon nanotubes (30 mg ml(-1)) to the working electrode increased the sensor sensitivity to 61.9 mM nA(-1) mm(-2), twice the value for the sensor without single-walled carbon nanotubes. A fabricated mediator-type biosensor sensor was used to perform real-time in vivo measurements. The sensor was implanted into the interstitial fluid of a fish eyeball, and detection was transmitted to a personal computer by a wireless potentiostat. Continuous measurement of the glucose concentration was possible for 78 hours. Stress was artificially applied to the fish during the measurement, and the change of blood glucose concentrations were observed. Our proposed sensor is applicable for effectively monitoring stress in free-swimming fish. PMID:22427105

  9. Effects of lithium (Li) on lithium-cuprous-oxide (Li-Cu2O) composite films grown by using electrochemical deposition for a PEC photoelectrode

    NASA Astrophysics Data System (ADS)

    Kim, Tae Gyoum; Ryu, Hyukhyun; Lee, Won-Jae

    2016-01-01

    In this study, Li-Cu2O composite films were grown on fluorine-doped tin-oxide (FTO) substrates by using the electrochemical deposition method. Various amounts of lithium (Li) were added to grow the Li-Cu2O composite films. We analyzed the morphology, structure, photocurrent density and photo-stability of the Li-Cu2O composite films by using various measurements such as field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) and potentiostat/galvanostat measurements, respectively. As a result, the highest XRD Cu2O (111)/ LiO (011) peak intensity ratio was obtained for the 10-wt% sample, which also had the highest photocurrent density value of -5.00 mA/cm2. The highest photocurrent density value for the 10-wt% sample was approximately 5 times greater than that of the 0-wt% sample. As shown by this result, we found that adding Li could improve the photocurrent values of Li-Cu2O composite films.

  10. Amperometric determination of acetylcholine-A neurotransmitter, by chitosan/gold-coated ferric oxide nanoparticles modified gold electrode.

    PubMed

    Chauhan, Nidhi; Pundir, C S

    2014-11-15

    An amperometric acetylcholine biosensor was constructed by co-immobilizing covalently, a mixture of acetylcholinesterase (AChE) and choline oxidase (ChO) onto nanocomposite of chitosan (CHIT)/gold-coated ferric oxide nanoparticles (Fe@AuNPs) electrodeposited onto surface of a Au electrode and using it as a working electrode, Ag/AgCl as reference electrode and Pt wire as auxiliary electrode connected through potentiostat. The biosensor is based on electrochemical measurement of H2O2 generated from oxidation of choline by immobilized ChO, which in turn is produced from hydrolysis of acetylcholine by immobilized AChE. The biosensor exhibited optimum response within 3s at +0.2V, pH 7.0 and 30°C. The enzyme electrode had a linear working range of 0.005-400 µM, with a detection limit of 0.005 µM for acetylcholine. The biosensor measured plasma acetylcholine in apparently healthy and persons suffering from Alzheimer's disease. The enzyme electrode was unaffected by a number of serum substances but lost 50% of its initial activity after its 100 uses over a period of 3 months, when stored at 4°C. PMID:24836212

  11. Integrated circuit-based electrochemical sensor for spatially resolved detection of redox-active metabolites in biofilms

    NASA Astrophysics Data System (ADS)

    Bellin, Daniel L.; Sakhtah, Hassan; Rosenstein, Jacob K.; Levine, Peter M.; Thimot, Jordan; Emmett, Kevin; Dietrich, Lars E. P.; Shepard, Kenneth L.

    2014-02-01

    Despite advances in monitoring spatiotemporal expression patterns of genes and proteins with fluorescent probes, direct detection of metabolites and small molecules remains challenging. A technique for spatially resolved detection of small molecules would benefit the study of redox-active metabolites that are produced by microbial biofilms and can affect their development. Here we present an integrated circuit-based electrochemical sensing platform featuring an array of working electrodes and parallel potentiostat channels. ‘Images’ over a 3.25 × 0.9 mm2 area can be captured with a diffusion-limited spatial resolution of 750 μm. We demonstrate that square wave voltammetry can be used to detect, identify and quantify (for concentrations as low as 2.6 μM) four distinct redox-active metabolites called phenazines. We characterize phenazine production in both wild-type and mutant Pseudomonas aeruginosa PA14 colony biofilms, and find correlations with fluorescent reporter imaging of phenazine biosynthetic gene expression.

  12. The effect of carbon nanotubes on the electrochemical hydrogen storage performance of LaNi 5 rare earth alloy

    NASA Astrophysics Data System (ADS)

    Fu, Xiaojuan; Zhang, Haiyan; Chen, Yiming; Li, Shunhua; Yi, Shuangping; Zhou, Chun; Li, Minghua; Zhu, Yanjuan; Chen, Jin

    2005-01-01

    We have investigated the electrochemical hydrogen storage performances of LaNi5 electrodes doped with carbon nanotubes (CNTs); the CNTs were prepared by chemical vapor deposition using a rare earth alloy as catalyst in a C2H2/H2 atmosphere. A three-electrode system was introduced; the above electrodes were used as the cathodes of the electronic cell, NiOOH/Ni(OH)2 as the anodes, and Hg/HgO as the reference electrodes. A 6 M aqueous KOH solution was introduced as the electrolyte. When the LaNi5 electrode was doped with 10% carbon nanotubes to its active material, it had a capacity of 407 mAh/g under the charge/discharge current density 200 and 100 mA/g, respectively. The discharge voltage limit was set as 0 V. The discharge trend is steadier while discharge plateau is improved to 0.875 V. Furthermore, we compared the electrochemical hydrogen storage capability of the LaNi5 electrodes doped with different ratios of CNTs (15%, 10%, 7% and 5%) under the same charge/discharge condition and found that the optimum doped quantity of CNTs is 10% in our experiment confines. The polarization peculiarity of each electrode was tested by the Transistor Potentiostat, which exhibited that LaNi5 electrodes doped with CNTs of different ratios have different electrochemical activation character.

  13. Discrete electrochemical transients of aluminium alloys generated by slurry jet impingement

    NASA Astrophysics Data System (ADS)

    Akiyama, Eiji; Stratmann, Martin; Hassel, Achim Walter

    2006-08-01

    Slurry impingement is a type of tribocorrosion resulting from simultaneous mechanical and electrochemical surface degradation. In order to understand the elementary process of slurry impingement and the effect of mechanical damage on passive films, electrochemical responses associated with passive film breakdown by particle impacts and following repassivation were measured during slurry impingement on Al and Al-1wt%Si alloy microelectrodes. Measurements were made using a slurry jet system which consists of a pump, a microelectrode, a potentiostat suited for measurements of fast transients of small currents and a high frequency data acquisition system. Current transients corresponding to separated single particle impacts have been successfully measured. The current transient sharply rises and gradually decays following a high field model of oxide growth. It is shown that pure Al repassivates faster after particle impact than the Al-1 wt% Si alloy. This type of erodent particle had an influence on the apparent repassivation rate of these electrodes, and both Al and Al-1 wt% Si alloy showed slower current decay after the impact of angular SiC particle than after the impact of spheroidal zirconia particle. The SiC particles made deep scars and scratches, and the zirconia particles made shallow depressions.

  14. Immobilization of lysine oxidase on a gold-platinum nanoparticles modified Au electrode for detection of lysine.

    PubMed

    Chauhan, N; Narang, J; Sunny; Pundir, C S

    2013-04-10

    A commercial lysine oxidase (LyOx) from Trichoderma viride was immobilized covalently onto gold nanoparticles (AuNPs) and platinum nanoparticles (PtNPs) electrodeposited onto Au electrode using 3-aminopropyltriethoxy silane (3-APTES) and glutaraldehyde cross linking chemistry. A lysine biosensor was fabricated using LyOx/3-APTES/AuNPs-PtNPs/Au electrode as a working electrode, Ag/AgCl (3M KCl) as standard electrode and Pt wire as auxiliary electrode connected through a potentiostat. The enzyme electrode was characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The cumulative effect of AuNPs and PtNPs showed excellent electrocatalytic activity at low applied potential for detection of H2O2, a product of LyOx reaction. The sensor showed its optimum response within 4s, when polarized at 0.2V vs. Ag/AgCl in 0.1M phosphate buffer, pH 7.5 at 30°C. The linear range and detection limit of the sensor were 1.0-600μM and 1.0μM (S/N=3), respectively. Biosensor measured lysine level in sera, milk and amino acid tablet, which correlated well with those by standard HPLC method. The enzyme electrode lost 50% of its initial activity after 200 uses over a period of 4 months. PMID:23540929

  15. Removal of tarnishing and roughness of copper surface by electropolishing treatment

    NASA Astrophysics Data System (ADS)

    Awad, A. M.; Ghany, N. A. Abdel; Dahy, T. M.

    2010-04-01

    Tarnishing and roughness of copper surface can be removed by electropolishing treatment (EP) imparting a bright and smooth surface at suitable conditions, e.g. current density, time, temperature, and viscosity. It was carried out by using an electrolytic cell containing phosphoric acid 55% as the electrolytic solution. Both copper working electrode and lead counter electrode, and reference electrode (SCE) were connected to a Potentiostat/Galvanostat to allow an electric current to pass through the solution. Some additives such as soluble starch, ethylene glycol, and methanol were added to reduce defects formed on the copper surface during EP process. The results showed that the highest gloss value was obtained by applying electric potential 1.5 V at the passive region of polarization curve. The surface was investigated after EP treatment, where SEM and EDX showed lower roughness in case of addition of both soluble starch and ethylene glycol more than methanol. Moreover, AFM analysis showed the lowest roughness in case of soluble starch more than other additives.

  16. 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.

  17. A fully implantable telemetry system for the chronic monitoring of brain tissue oxygen in freely moving rats.

    PubMed

    Russell, David M; Garry, Emer M; Taberner, Andrew J; Barrett, Carolyn J; Paton, Julian F R; Budgett, David M; Malpas, Simon C

    2012-03-15

    The ability to monitor tissue oxygen concentration in a specific region of the brain in a freely moving animal could provide a new paradigm in neuroscience research. We have developed a fully implantable telemetry system for the continuous and chronic recording of brain tissue oxygen (PO(2,BR)) in conscious animals. A telemetry system with a sampling rate of 2kHz was combined with a miniaturized potentiostat to amperiometrically detect oxygen concentration with carbon paste electrodes. Wireless power was employed to recharge the telemeter battery transcutaneously for potential lifetime monitoring. Rats were implanted with the telemeter in the peritoneal cavity and electrodes stereotaxically implanted into the brain (striatum or medulla oblongata). While the animals were living in their home cages the sensitivity to changes in oxygen was validated by repeatedly altering the inspired oxygen (10%, 100%, respectively) or a pharmacological stimulus (carbonic anhydrase inhibitor: acetazolamide 50mg/kg IP). Basal level of PO(2,BR) was monitored for 3weeks and showed good overall stability and good correlation to movement such as grooming. During hypoxia, PO(2,BR) decreased significantly by -51%±2% from baseline, whereas it increased by 34%±3% during hyperoxia. Following the systemic administration of acetazolamide, PO(2,BR) increased by 38%±4%. We propose this new technology provides a robust method to measure changes in oxygen concentration in specific areas of the brain, in conscious freely moving rats. The ability to track long term changes with disease progression or drug treatment may be enabled. PMID:22123353

  18. Electrochemical Fractionation of Molybdenum Stable Isotopes

    NASA Astrophysics Data System (ADS)

    Crawford, J.; Black, J.; Wasylenki, L.; Gordon, G.; Anbar, A.; Kavner, A.

    2008-12-01

    Stable isotope signatures were measured from Molybdenum (Mo) electrodeposited from aqueous solution. As potential varied from -1.35 V to -2.00 V (relative to Ag/AgCl), fractionation decreases from Δ97/95Mo = -1.3 ‰ to -0.9 ‰ (Δ97/95Mo defined as the difference in the 97Mo/95Mo ratio of deposited Mo relative to aqueous Mo). Natural variations of δ97/95Mo span a range of ~ 3 ‰ [Barling, J. and Anbar, A. D., EPSL. 2004, 217: 315], therefore, charge transfer driven fractionation may be responsible for some of the observed variation in Mo stable isotope geochemistry. Following previous approaches with Fe and Zn [Kavner, A. et al. Geochim. Cosmochim. Acta. 2005, 69: 2971; 2008, 72: 1731], Mo was plated in a three-electrode cell from a neutral to slightly alkaline solution (pH ~ 8.7). Voltage was held constant during electrodeposition using an Autolab Potentiostat. In all experiments, less than 0.5 % of the Mo was deposited, which insures that the plating reservoir remains at an approximately constant isotopic composition. Plated Mo was then recovered in acid, and the isotopic composition of samples and stock solutions were measured using a Thermo Scientific Neptune MC-ICP-MS. These experiments show that the redox process induces an isotopic signature with respect to the starting material, with a trend showing that fractionation decreases as a function of applied voltage.

  19. Microchip electrophoresis with amperometric detection for the study of the generation of nitric oxide by NONOate salts.

    PubMed

    Gunasekara, Dulan B; Hulvey, Matthew K; Lunte, Susan M; da Silva, José Alberto Fracassi

    2012-06-01

    Microchip electrophoresis (ME) with electrochemical detection was used to monitor nitric oxide (NO) production from diethylammonium (Z)-1-(N,N-diethylamino)diazen-1-ium-1,2-diolate (DEA/NO) and 1-(hydroxyl-NNO-azoxy)-L-proline disodium salt (PROLI/NO). NO was generated through acid hydrolysis of these NONOate salts. The products of acid hydrolysis were introduced into a 5-cm separation channel using gated injection. The separation was accomplished using reverse polarity and a background electrolyte consisting of 10 mM boric acid and 2 mM tetradecyltrimethylammonium bromide, pH 11. Electrochemical detection was performed using an isolated potentiostat in an in-channel configuration. Potentials applied to the working electrode, typically higher than +1.0 V vs. Ag/AgCl, allowed the direct detection of nitrite, NO, DEA/NO, and PROLI/NO. Baseline resolution was achieved for the separation of PROLI/NO and NO while resolution between DEA/NO and NO was poor (1.0 ± 0.2). Nitrite was present in all samples tested. PMID:22415023

  20. A Portable Liquid Chromatograph with a Battery-operated Compact Electroosmotic Pump and a Microfluidic Chip Device with a Reversed Phase Packed Column.

    PubMed

    Ishida, Akihiko; Fujii, Mitsutaka; Fujimoto, Takehiro; Sasaki, Shunsuke; Yanagisawa, Ichiro; Tani, Hirofumi; Tokeshi, Manabu

    2015-01-01

    A compact and lightweight liquid chromatography system is presented with overall dimensions of 26 cm width × 18 cm length × 21 cm height and weight of 2 kg. This system comprises a battery-operated compact electroosmotic pump, a manual injector, a microfluidic chip device containing a packed column and an electrochemical detector, and a USB bus-powered potentiostat. The pumping system was designed for microfluidic-based reversed-phase liquid chromatography in which an electroosmotically generated water stream pushes the mobile phase via a diaphragm for the output. The flow rate ranged from 0 to 10 μL/min and had a high degree of precision. The pumping system operated continuously for over 24 h with dry batteries. The column formed in the microfluidic device was packed with 3-μm ODS particles with a length of 30 mm and a diameter of 0.8 mm. The results presented herein demonstrate the performance of the pumping system and the column using alkylphenols, catecholamine, catechin, and amino acids. PMID:26561261

  1. Electrochemical monitoring of the metabolic activity of mycobacteria in culture.

    PubMed

    Rodríguez, Jimmy; Ramírez, Ana-S; Suárez, Marco-Fidel; Soto, Carlos-Yesid

    2012-06-01

    Mycobacterial metabolic activity is typically measured using time-consuming manual methods based on nutrient consumption, nucleic acid synthesis or reduction of tetrazolium salts. In this study, we propose much simpler electrochemical methods for continuous monitoring of the metabolic activity of mycobacteria in culture. Chronoamperometry and chronopotentiometry were used to detect metabolic activity of both slow-growing and fast-growing mycobacteria using a potentiostat with 2D-electrochemical cell. Electrochemical measurements were able to detect statistically significant differences in the metabolic activity of approximately 10(7) mycobacteria in different growth conditions, within less than 24 h of mycobacterial culture. The metabolic activity of mycobacteria measured by the used electrochemical methods correlated well with changes in general respiratory conditions within the cells as it was evaluated by different biochemical tests. Chronoamperometry and chronopotentiometry allowed measurement of mycobacterial metabolic activity without invasive chemical reactions, at minimal bacterial load and when metabolic response of mycobacteria occurs quickly. The proposed methodology is simple, rapid and cost-effective, and it is expected that both in vitro and in vivo metabolic activity of human mycobacterial pathogens as Mycobacterium tuberculosis can be measured when the implementation of this method to analyze virulent strains is adapted. PMID:22453520

  2. Fabrication of vertically aligned Pd nanowire array in AAO template by electrodeposition using neutral electrolyte

    NASA Astrophysics Data System (ADS)

    Taşaltın, Nevin; Öztürk, Sadullah; Kılınç, Necmettin; Yüzer, Hayrettin; Öztürk, Zafer Ziya

    2010-07-01

    A vertically aligned Pd nanowire array was successfully fabricated on an Au/Ti substrate using an anodic aluminum oxide (AAO) template by a direct voltage electrodeposition method at room temperature using diluted neutral electrolyte. The fabrication of Pd nanowires was controlled by analyzing the current-time transient during electrodeposition using potentiostat. The AAO template and the Pd nanowires were characterized by scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) methods and X-Ray diffraction (XRD). It was observed that the Pd nanowire array was standing freely on an Au-coated Ti substrate after removing the AAO template in a relatively large area of about 5 cm2, approximately 50 nm in diameter and 2.5 μm in length with a high aspect ratio. The nucleation rate and the number of atoms in the critical nucleus were determined from the analysis of current transients. Pd nuclei density was calculated as 3.55 × 108 cm-2. Usage of diluted neutral electrolyte enables slower growing of Pd nanowires owing to increase in the electrodeposition potential and thus obtained Pd nanowires have higher crystallinity with lower dislocations. In fact, this high crystallinity of Pd nanowires provides them positive effect for sensor performances especially.

  3. Room-temperature epitaxial electrodeposition of single-crystalline germanium nanowires at the wafer scale from an aqueous solution.

    PubMed

    Fahrenkrug, Eli; Gu, Junsi; Jeon, Sunyeol; Veneman, P Alexander; Goldman, Rachel S; Maldonado, Stephen

    2014-02-12

    Direct epitaxial growth of single-crystalline germanium (Ge) nanowires at room temperature has been performed through an electrodeposition process on conductive wafers immersed in an aqueous bath. The crystal growth is based on an electrochemical liquid-liquid-solid (ec-LLS) process involving the electroreduction of dissolved GeO2(aq) in water at isolated liquid gallium (Ga) nanodroplet electrodes resting on single-crystalline Ge or Si supports. Ge nanowires were electrodeposited on the wafer scale (>10 cm(2)) using only common glassware and a digital potentiostat. High-resolution electron micrographs and electron diffraction patterns collected from cross sections of individual substrate-nanowire contacts in addition to scanning electron micrographs of the orientation of nanowires across entire films on substrates with different crystalline orientations, supported the notion of epitaxial nanowire growth. Energy dispersive spectroscopic elemental mapping of single nanowires indicated the Ga(l) nanodroplet remains affixed to the tip of the growing nanowire throughout the nanowire electrodeposition process. Current-voltage responses measured across many individual nanowires yielded reproducible resistance values. The presented data cumulatively show epitaxial growth of covalent group IV nanowires is possible from the reduction of a dissolved oxide under purely benchtop conditions. PMID:24417670

  4. Effects of Potential and Mechanical Stimulation on Oxidation of Tantalum During Electrochemical Mechanical Polishing

    NASA Astrophysics Data System (ADS)

    Gao, F.; Liang, Hong

    2012-03-01

    Metal oxidation under stress plays a significant role in many industrial applications, particularly in chemical mechanical polishing (CMP). Here we report effects of mechanical stimulation on tantalum (Ta) oxidation during CMP. A tantalum surface was polished at various anodic potentials and under different mechanical forces. A potentiostat was used to measure the anodic reaction current during electrochemical mechanical polishing (ECMP). The material removal rate (MRR) measured using atomic force microscopy (AFM) was compared with that calculated using Faraday's law. Relationship was linked (or established) between the anodic potential and a mechanical force. The MRR was a second-order polynomial function of potential at constant mechanical force, followed by a logarithmic function. It was found that more suboxides were present at extreme potentials (low and high), while substantial pentoxide was generated under intermediate potentials. A model is proposed to explain the oxidation process of Ta during ECMP. The oxidation of Ta was a function of the anodic potential and mechanical force. The ex situ method used in this study fulfilled the in situ observation on Ta oxidation in polishing. Additionally, this technique can be used to investigate oxidation of other metals.

  5. High-resolution neutron powder diffractometer SPODI at research reactor FRM II

    NASA Astrophysics Data System (ADS)

    Hoelzel, M.; Senyshyn, A.; Juenke, N.; Boysen, H.; Schmahl, W.; Fuess, H.

    2012-03-01

    SPODI is a high-resolution thermal neutron diffractometer at the research reactor Heinz Maier-Leibnitz (FRM II) especially dedicated to structural studies of complex systems. Unique features like a very large monochromator take-off angle of 155° and a 5 m monochromator-sample distance in its standard configuration achieve both high-resolution and a good profile shape for a broad scattering angle range. Two dimensional data are collected by an array of 80 vertical position sensitive 3He detectors. SPODI is well suited for studies of complex structural and magnetic order and disorder phenomena at non-ambient conditions. In addition to standard sample environment facilities (cryostats, furnaces, magnet) specific devices (rotatable load frame, cell for electric fields, multichannel potentiostat) were developed. Thus the characterisation of functional materials at in-operando conditions can be achieved. In this contribution the details of the design and present performance of the instrument are reported along with its specifications. A new concept for data reduction using a 2 θ dependent variable height for the intensity integration along the Debye-Scherrer lines is introduced.

  6. Design of a high-speed electrochemical scanning tunneling microscope.

    PubMed

    Yanson, Y I; Schenkel, F; Rost, M J

    2013-02-01

    In this paper, we present a bottom-up approach to designing and constructing a high-speed electrochemical scanning tunneling microscope (EC-STM). Using finite element analysis (FEA) calculations of the frequency response of the whole mechanical loop of the STM, we analyzed several geometries to find the most stable one that could facilitate fast scanning. To test the FEA results, we conducted measurements of the vibration amplitudes using a prototype STM setup. Based on the FEA analysis and the measurement results, we identified the potentially most disturbing vibration modes that could impair fast scanning. By modifying the design of some parts of the EC-STM, we reduced the amplitudes as well as increased the resonance frequencies of these modes. Additionally, we designed and constructed an electrochemical flow-cell that allows STM imaging in a flowing electrolyte, and built a bi-potentiostat to achieve electrochemical potential control during the measurements. Finally, we present STM images acquired during high-speed imaging in air as well as in an electrochemical environment using our newly-developed EC-STM. PMID:23464213

  7. Construction of an uricase nanoparticles modified au electrode for amperometric determination of uric acid.

    PubMed

    Chauhan, Nidhi; Kumar, Arun; Pundir, C S

    2014-10-01

    A method is described for preparation of uricase nanoparticles (100 nm in size) and their direct immobilization onto the Au electrode. The enzyme electrode along with Ag/AgCl as reference and Pt as auxiliary electrode were connected through potentiostat/galvanostat to construct an amperometric uric acid biosensor. The enzyme electrode was characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, and electrochemical impedance spectroscopy (EIS). The enzyme electrode detected uric acid level as low as 5.0 μM at a signal-to-noise ratio of 3, within 7 s at pH 8.5 and 40 °C. The biosensor showed a linear working range, 0.005 to 0.8 mM for uric acid with a sensitivity of 0.03 mA μM(-1) cm(-2). The biosensor was evaluated. The biosensor lost only 15 % of its initial activity over a period of 7 months, when stored at 4 °C. The fabricated biosensor was successfully employed for determination of uric acid in human serum and urine. PMID:25141984

  8. Miniaturized electrochemical system for cholinesterase inhibitor detection.

    PubMed

    Veloso, Anthony J; Nagy, Paul M; Zhang, Biao; Dhar, Devjani; Liang, Anqi; Ibrahim, Tarek; Mikhaylichenko, Svetlana; Aubert, Isabelle; Kerman, Kagan

    2013-04-24

    The utility of a simple, low-cost detection platform for label-free electrochemical characterization of acetylcholinesterase (AChE) inhibition is demonstrated as a potential tool for screening of small-molecule therapeutic agents for Alzheimer's disease (AD). Technique validation was performed against the standard Ellman's colorimetric assay using the clinically established cholinesterase inhibitor (ChEI), Donepezil (Aricept(®)). Electrochemical measurements were obtained by differential pulse voltammetry (DPV) performed using a portable potentiostat system for detection of the enzymatic product, thiocholine (TCh), by direct oxidation on unmodified gold screen-printed electrodes. The IC50 profiles for Donepezil measured in vitro were found to be comparable between both colorimetric and electrochemical detection methods for the analysis of purified human erythrocyte-derived AChE (28±7 nM by DPV; 26±8 nM by Ellman's method). The selectivity of this unmodified electrode system was compared to a range of biological sulfur-containing compounds including cysteine, homocysteine, glutathione and methionine as well as ascorbic acid. Preliminary studies also demonstrated the potential applicability of this electrochemical technique for the analysis of Donepezil in crude cholinesterase samples from anterior cortex homogenates of C57BL/6J mice. PMID:23567119

  9. Virtual electrochemical nitric oxide analyzer using copper, zinc superoxide dismutase immobilized on carbon nanotubes in polypyrrole matrix.

    PubMed

    Madasamy, Thangamuthu; Pandiaraj, Manickam; Balamurugan, Murugesan; Karnewar, Santosh; Benjamin, Alby Robson; Venkatesh, Krishna Arun; Vairamani, Kanagavel; Kotamraju, Srigiridhar; Karunakaran, Chandran

    2012-10-15

    In this work, we have designed and developed a novel and cost effective virtual electrochemical analyzer for the measurement of NO in exhaled breath and from hydrogen peroxide stimulated endothelial cells using home-made potentiostat. Here, data acquisition system (NI MyDAQ) was used to acquire the data from the electrochemical oxidation of NO mediated by copper, zinc superoxide dismutase (Cu,ZnSOD). The electrochemical control programs (graphical user-interface software) were developed using LabVIEW 10.0 to sweep the potential, acquire the current response and process the acquired current signal. The Cu,ZnSOD (SOD1) immobilized on the carbon nanotubes in polypyrrole modified platinum electrode was used as the NO biosensor. The electrochemical behavior of the SOD1 modified electrode exhibited the characteristic quasi-reversible redox peak at the potential, +0.06 V vs. Ag/AgCl. The biological interferences were eliminated by nafion coated SOD1 electrode and then NO was measured selectively. Further, this biosensor showed a wide linear range of response over the concentration of NO from 0.1 μM to 1 mM with a detection limit of 0.1 μM and high sensitivity of 1.1 μA μM(-1). The electroanalytical results obtained here using the developed virtual electrochemical instrument were also compared with the standard cyclic voltammetry instrument and found in agreement with each other. PMID:23141325

  10. Properties of the nano-thick Pt/W bilayered catalytic layer employed dye sensitized solar cells

    NASA Astrophysics Data System (ADS)

    Noh, Yunyoung; Song, Ohsung

    2014-05-01

    A Pt/W bilayered catalytic layer on a flat glass substrate was used as a counter electrode to improve the energy conversion efficiency of a dye-sensitized solar cell device with the structure of 0.45 cm2 effective area of glass/FTO/blocking layer/TiO2/N719 (dye)/electrolyte/50 nm Pt/50 nm W/glass. For comparison, 100 nm-thick Pt and W counter electrodes on flat glass substrates were also prepared using the same procedure. The photovoltaic properties, such as the short circuit current density, open circuit voltage, fill factor, energy conversion efficiency and impedance were characterized using a solar simulator and potentiostat. The phases and microstructures of the catalytic layers were examined by x-ray diffraction and field emission electron microscopy. The measured energy conversion efficiencies of the dye-sensitized solar cell devices with Pt only and Pt/W bilayer counter electrodes were 4.60% and 6.54%, respectively. The interface resistance at the interface between the counter electrode and electrolyte decreased when a Pt/W bilayered thin film was applied. The increase in efficiency resulted from the effect of compressive strain field formed by the intermetallic layer of Pt2W at Pt and W layer interface. This suggests that the use of Pt/W bilayered catalytic layers improves the efficiency of the dye-sensitized solar cells compared to those using the conventional Pt layers.

  11. Amperometric bienzyme screen-printed biosensor for the determination of leucine.

    PubMed

    Labroo, Pratima; Cui, Yue

    2014-01-01

    Leucine plays an important role in protein synthesis, brain functions, building muscle mass, and helping the body when it undergoes stress. Here, we report a new amperometric bienzyme screen-printed biosensor for the determination of leucine, by coimmobilizing p-hydroxybenzoate hydroxylase (HBH) and leucine dehydrogenase (LDH) on a screen-printed electrode with NADP(+) and p-hydroxybenzoate as the cofactors. The detection principle of the sensor is that LDH catalyzes the specific dehydrogenation of leucine by using NADP(+) as a cofactor. The product, NADPH, triggers the hydroxylation of p-hydroxybenzoate by HBH in the presence of oxygen to produce 3,4-dihydroxybenzoate, which results in a change in electron concentration at the working carbon electrode, which is detected by the potentiostat. The sensor shows a linear detection range between 10 and 600 μM with a detection limit of 2 μM. The response is reproducible and has a fast measuring time of 5-10 s after the addition of a given concentration of leucine. PMID:24220759

  12. Tyrosinase conjugated reduced graphene oxide based biointerface for bisphenol A sensor.

    PubMed

    Reza, K Kamil; Ali, Md Azahar; Srivastava, Saurabh; Agrawal, Ved Varun; Biradar, A M

    2015-12-15

    We have fabricated a nanocomposite of reduced graphene oxide (rGO) sheets and chitosan (Cn) polymer based highly sensitive electrochemical biosensor for detection of bisphenol A (BPA). The two-dimensional structure and chemical functionality of rGO and Cn provide an excellent electrode surface for loading of tyrosinase enzyme molecules. This rGO-Cn nanocomposite is capable of effectively utilizing their superior conductivity, larger effective surface area and superior electrochemical performance due to its synergistic effect between rGO and Cn. The structural, morphological and electrochemical characterizations of nanocomposite sheets have been performed by electron microscopy, X-ray diffraction, FTIR and Potentiostat/Galvanostat techniques. This fabricated biosensor is sensitive to nanomolar (0.74 nM) concentration of BPA and detection time is 10s compared to conventional BPA ELISA kit (0.3 µg/L and 2.5h). The rGO-Cn based biosensor exhibits a higher sensitivity (83.3 µA nM(-1) cm(-2)), wider linearity (0.01-50 µM) with good selectivity towards BPA. This biosensor is capable to quantify real sample of BPA using packaged drinking water bottles. This rGO-Cn nanocomposite sheets emerges as a potential electrode material for detection of other estrogenic substrate. PMID:26201981

  13. The azo dye Disperse Red 13 and its oxidation and reduction products showed mutagenic potential.

    PubMed

    Chequer, Farah Maria Drumond; Lizier, Thiago Mescoloto; de Felício, Rafael; Zanoni, Maria Valnice Boldrin; Debonsi, Hosana Maria; Lopes, Norberto Peporine; de Oliveira, Danielle Palma

    2015-10-01

    Common water pollutants, azo dyes and their degradation products have frequently shown toxicity, including carcinogenic and mutagenic effects, and can induce serious damage in aquatic organisms and humans. In the present study, the mutagenic potential of the azo dye Disperse Red 13 (DR13) was first evaluated using the Micronucleus Assay in human lymphocytes. Subsequently, in order to mimic hepatic biotransformation, controlled potential electrolysis was carried out with a DR13 solution using a Potentiostat/Galvanostat. In addition, a DR13 solution was oxidized using S9 (homogenate of rat liver cells). DR13 oxidation and the reduction products were identified using HPLC-DAD and GC/MS, and their mutagenic potential investigated by way of a Salmonella/microsome assay using TA98 and YG1041 strains, with no S9. The original azo dye DR13 induced chromosomal damage in human lymphocytes, and the respective oxidation and reduction products also showed mutagenic activity, as detected by the Salmonella/microsome assay. Furthermore sulfate 2-[(4-aminophenyl)ethylamino]-ethanol monohydrate, 2-chloro-4-nitro-benzamine, 4-nitro-benzamine and 2-(ethylphenylamine)-ethanol were identified as products of the DR13 reduction/oxidation reactions. Thus it was concluded that the contamination of water effluents with DR13 is a health risk not only due to the dye itself, but also due to the possibility of drinking contaminated water, considering the harmful compounds that can be produced after hepatic biotransformation. PMID:26247324

  14. Direct electrochemical sensor for label-free DNA detection based on zero current potentiometry.

    PubMed

    Wu, Nai-ying; Gao, Wei; He, Xu-lun; Chang, Zhu; Xu, Mao-tian

    2013-01-15

    A direct electrochemical DNA biosensor based on zero current potentiometry was fabricated by immobilization of ssDNA onto gold nanoparticles (AuNPs) coated pencil graphite electrode (PGE). One ssDNA/AuNPs/PGE was connected in series between clips of working and counter electrodes of a potentiostat, and then immersed into the solution together with a reference electrode, establishing a novel DNA biosensor for specific DNA detection. The variation of zero current potential difference (ΔE(zcp)) before and after hybridization of the self-assembled probe DNA with the target DNA was used as a signal to characterize and quantify the target DNA sequence. The whole DNA biosensor fabrication process was characterized by cyclic voltammetry and electrochemical impedance spectroscopy with the use of ferricyanide as an electrochemical redox indicator. Under the optimized conditions, ΔE(zcp) was linear with the concentrations of the complementary target DNA in the range from 10nM to 1μM, with a detection limit of 6.9nM. The DNA biosensor showed a good reproducibility and selectivity. Prepared DNA biosensor is facile and sensitive, and it eliminates the need of using exogenous reagents to monitor the oligonucleotides hybridization. PMID:22884003

  15. Microbiologically induced corrosive properties of the titanium surface.

    PubMed

    Fukushima, A; Mayanagi, G; Nakajo, K; Sasaki, K; Takahashi, N

    2014-05-01

    Corrosion of titanium is the major concern when it is used for dental treatment. This study aimed to investigate the mechanism of the microbiologically induced corrosive properties of titanium. An experimental well was made of polymethyl methacrylate with pure titanium at the bottom. Viable or killed cells of Streptococcus mutans were packed into the well, and pH at the bacteria-titanium interface was monitored with and without glucose. Before and after 90-minute incubation, the electrochemical behavior on the titanium surface was measured by means of a potentiostat. The oxygen concentration under bacterial cells was monitored with oxygen-sensitive fluorescent film. The amount of titanium eluted was measured by inductively coupled plasma-mass spectrometry. The corrosion current and passive current under killed cells were low and stable during 90 min, while those under viable cells increased, regardless of the glucose-induced pH fall. The polarization resistance and oxygen concentration under killed cells were high and stable, while those under viable cells decreased. No elution of titanium was detected. Viable bacterial cells may form 'oxygen concentration cells' through metabolism-coupled oxygen consumption and subsequently induce corrosive properties of the titanium surface. PMID:24554541

  16. Disposable electrochemical sensor to evaluate the phytoremediation of the aquatic plant Lemna minor L. toward Pb(2+) and/or Cd(2+).

    PubMed

    Neagu, Daniela; Arduini, Fabiana; Quintana, Josefina Calvo; Di Cori, Patrizia; Forni, Cinzia; Moscone, Danila

    2014-07-01

    In this work a miniaturized and disposable electrochemical sensor was developed to evaluate the cadmium and lead ion phytoremediation potential by the floating aquatic macrophyte Lemna minor L. The sensor is based on a screen-printed electrode modified "in-situ" with bismuth film, which is more environmentally friendly than the mercury-based sensor usually adopted for lead and cadmium ion detection. The sensor was coupled with a portable potentiostat for the simultaneous measurement of cadmium and lead ions by stripping analysis. The optimized analytical system allows the simultaneous detection of both heavy metals at the ppb level (LOD equal to 0.3 and 2 ppb for lead and cadmium ions, respectively) with the advantage of using a miniaturized and cost-effective system. The sensor was then applied for the evaluation of Pb(2+) or/and Cd(2+) uptake by measuring the amount of the heavy metals both in growth medium and in plant tissues during 1 week experiments. In this way, the use of Lemna minor coupled with a portable electrochemical sensor allows the set up of a model system able both to remove the heavy metals and to measure "in-situ" the magnitude of heavy metal removal. PMID:24899412

  17. Rapid, Single-Cell Electrochemical Detection of Mycobacterium tuberculosis Using Colloidal Gold Nanoparticles.

    PubMed

    Ng, Benjamin Y C; Xiao, Wei; West, Nicholas P; Wee, Eugene J H; Wang, Yuling; Trau, Matt

    2015-10-20

    Tuberculosis (TB) remains a global health threat, with over a third of the world population suffering from the disease, and 1.5 million deaths due to the disease in 2013 alone. Despite significant advances in TB detection strategies in recent years, a bigger push toward detecting TB in the shortest and easiest way possible at the point-of-care (POC) is still in demand. To this end, we have designed a simple yet rapid and sensitive bioassay that detects Mtb DNA electrochemically using colloidal gold nanoparticles. This assay couples rapid isothermal amplification of target DNA that is specific to Mtb with gold nanoparticle electrochemistry on disposable screen printed carbon electrodes. The assay is capable of detecting a positive differential pulse voltammetry (DPV) response from as low as 1 CFU of Mtb bacilli DNA input material, having shown its exquisite sensitivity over a conventional gel based readout. The translation of our assay onto a portable potentiostat was also demonstrated, with promising results. We believe that our assay has significant potential for translation into broader bioassay applications or development as a POC diagnostic tool. PMID:26382883

  18. Development of an on-animal separation-based sensor for monitoring drug metabolism in freely roaming sheep.

    PubMed

    Scott, David E; Willis, Sean D; Gabbert, Seth; Johnson, David; Naylor, Erik; Janle, Elsa M; Krichevsky, Janice E; Lunte, Craig E; Lunte, Susan M

    2015-06-01

    The development of an on-animal separation-based sensor that can be employed for monitoring drug metabolism in a freely roaming sheep is described. The system consists of microdialysis sampling coupled to microchip electrophoresis with electrochemical detection (MD-ME-EC). Separations were accomplished using an all-glass chip with integrated platinum working and reference electrodes. Discrete samples from the microdialysis flow were introduced into the electrophoresis chip using a flow-gated injection approach. Electrochemical detection was accomplished in-channel using a two-electrode isolated potentiostat. Nitrite was separated by microchip electrophoresis using reverse polarity and a run buffer consisting of 50 mM phosphate at pH 7.4. The entire system was under telemetry control. The system was first tested with rats to monitor the production of nitrite following perfusion of nitroglycerin into the subdermal tissue using a linear probe. The data acquired using the on-line MD-ME-EC system were compared to those obtained by off-line analysis using liquid chromatography with electrochemical detection (LC-EC), using a second microdialysis probe implanted parallel to the first probe in the same animal. The MD-ME-EC device was then used on-animal to monitor the subdermal metabolism of nitroglycerin in sheep. The ultimate goal is to use this device to simultaneously monitor drug metabolism and behavior in a freely roaming animal. PMID:25697221

  19. Microelectrospotting as a new method for electrosynthesis of surface-imprinted polymer microarrays for protein recognition.

    PubMed

    Bosserdt, Maria; Erdőssy, Júlia; Lautner, Gergely; Witt, Julia; Köhler, Katja; Gajovic-Eichelmann, Nenad; Yarman, Aysu; Wittstock, Gunther; Scheller, Frieder W; Gyurcsányi, Róbert E

    2015-11-15

    Here we introduce microelectrospotting as a new approach for preparation of protein-selective molecularly imprinted polymer microarrays on bare gold SPR imaging chips. During electrospotting both the gold chip and the spotting tip are electrically connected to a potentiostat as working and counter electrodes, respectively. The spotting pin encloses the monomer-template protein cocktail that upon contacting the gold surface is in-situ electropolymerized resulting in surface confined polymer spots of ca. 500 µm diameter. By repeating this procedure at preprogrammed locations for various composition monomer-template mixtures microarrays of nanometer-thin surface-imprinted films are generated in a controlled manner. We show that the removal and rebinding kinetics of the template and various potential interferents to such microarrays can be monitored in real-time and multiplexed manner by SPR imaging. The proof of principle for microelectrospotting of electrically insulating surface-imprinted films is made by using scopoletin as monomer and ferritin as protein template. It is shown that microelectrospotting in combination with SPR imaging can offer a versatile platform for label-free and enhanced throughput optimization of the molecularly imprinted polymers for protein recognition and for their analytical application. PMID:26056955

  20. A low power sensor signal processing circuit for implantable biosensor applications

    NASA Astrophysics Data System (ADS)

    Zhang, Mo; Haider, Mohammad R.; Huque, Mohammad A.; Adeeb, Mohammad A.; Rahman, Shaela; Islam, Syed K.

    2007-04-01

    A low power sensor read-out circuit has been implemented in 0.35 µm CMOS technology that consumes only 400 µW of power and occupies an area of 0.66 mm2. The circuit is capable of converting the current signal from any generic biosensor into an amplitude shift keying (ASK) signal. The on-chip potentiostat biases the chemical sensor electrodes to create the sensor current which is then integrated and buffered to generate a square wave with a frequency proportional to the sensor current level. A programmable frequency divider is incorporated to fix the ASK envelope frequency to be inbetween 20 Hz and 20 kHz, which is within the audible range of human hearing. The entire transmitter block operates with a supply voltage as low as 1.5 V, and it can be easily powered up by an external RF source. Test results emulate the simulation results with good agreement and corroborate the efficacy of the designed system.

  1. Electrodeposited nickel-cobalt composite coating containing MoS 2

    NASA Astrophysics Data System (ADS)

    Shi, Lei; Sun, Chufeng; Liu, Weimin

    2008-08-01

    Ni-Co/MoS 2 composite coatings were prepared by electrodeposition in a Ni-Co plating bath containing nano-sized MoS 2 particles to be co-deposited. The polarization behavior of the composite plating bath was examined on a PAR-273A potentiostat/galvanostat device. The friction and wear behaviors of the Ni-Co/MoS 2 composite coatings were evaluated with UMT-2MT test rig in a ball-on-disk contact mode. The morphologies of the original and worn surfaces of the composite coatings were observed on scanning electron microscope (SEM). It was found that the introduction of MoS 2 nano-particulates in the electrolyte caused the shift towards larger negatives of the reduction potential of the Ni-Co alloy coating, and the co-deposited MoS 2 showed no significant effect on the electrodeposition process of the Ni-Co alloy coating. However, the co-deposited MoS 2 led to changes in the surface morphology and structure of the composite coating as well. Namely, the peak width of the Ni-Co solid solution for the composite coating is broader as compared to that of the Ni-Co alloy coating. The co-deposited MoS 2 particulates were uniformly distributed in the Ni-Co matrix and contributed to increase tribological properties of the Ni-Co alloy coating.

  2. Miniaturized voltammetric stripping on screen printed gold electrodes for field determination of copper in atmospheric deposition.

    PubMed

    Rueda-Holgado, F; Bernalte, E; Palomo-Marín, M R; Calvo-Blázquez, L; Cereceda-Balic, F; Pinilla-Gil, E

    2012-11-15

    The applicability of commercial screen-printed gold electrodes (SPGEs) connected to a portable potentiostat and a laptop has been explored to optimize a new square wave anodic stripping voltammetric method for on-site determination of soluble Cu(II) in atmospheric deposition samples taken around an industrial complex. Electrode conditioning procedures, chemical and instrumental variables have been optimized to develop a reliable method capable of measuring dissolved copper with a detection limit of 3.7 ng mL(-1), useful for pollution monitoring or screening purposes. The proposed method was tested with the SLRS-5 River Water for Trace Metals (recoveries 109.9-113.1%) and the SPS-SW2 Batch 121 Elements in Surface Waters (recoveries 93.2-97.6%). The method was applied to soluble Cu(II) measurement in liquid samples taken by a total atmospheric deposition collector modified with a quartz filter for soluble and insoluble elemental speciation. The voltammetric measurements on field samples were tested in the lab by a reference ICP-MS method, with good agreement. The proposed method proved capability for field operation during a two weeks monitoring campaign. PMID:23158345

  3. Electrochemical sensing method for point-of-care cortisol detection in human immunodeficiency virus-infected patients.

    PubMed

    Kaushik, Ajeet; Yndart, Adriana; Jayant, Rahul Dev; Sagar, Vidya; Atluri, Venkata; Bhansali, Shekhar; Nair, Madhavan

    2015-01-01

    A novel electrochemical sensing method was devised for the first time to detect plasma cortisol, a potential psychological stress biomarker, in human immunodeficiency virus (HIV)-positive subjects. A miniaturized potentiostat (reconfigured LMP91000 chip) interfaced with a microfluidic manifold containing a cortisol immunosensor was employed to demonstrate electrochemical cortisol sensing. This fully integrated and optimized electrochemical sensing device exhibited a wide cortisol-detection range from 10 pg/mL to 500 ng/mL, a low detection limit of 10 pg/mL, and sensitivity of 5.8 μA (pg mL)(-1), with a regression coefficient of 0.995. This cortisol-selective sensing system was employed to estimate plasma cortisol in ten samples from HIV patients. The electrochemical cortisol-sensing performance was validated using an enzyme-linked immunosorbent assay technique. The results obtained using both methodologies were comparable within 2%-5% variation. The information related to psychological stress of HIV patients can be correlated with disease-progression parameters to optimize diagnosis, therapeutic, and personalized health monitoring. PMID:25632229

  4. Effects of Zn amount on the properties of Zn-Zu2O composite films grown for PEC photoelectrodes by using electrochemical deposition

    NASA Astrophysics Data System (ADS)

    Kim, Tae Gyoum; Lee, Hu Joong; Ryu, Hyukhyun; Lee, Won-Jae

    2015-10-01

    In this study, Zn-Cu2O composite films were grown on fluorine-doped tin-oxide (FTO) substrates by using the electrochemical deposition method. Various amounts of Zinc (Zn) were added to grow the Zn-Cu2O composite films. We analyzed the morphological, structural, optical energy band gap and photocurrent density properties of the Zn-Cu2O composite films by using various measurements such as field-emission scanning electron microscope (FE-SEM), X-ray diffraction (XRD), UV-visible spectrophotometry and potentiostat/galvanostat measurements, respectively. As a result, the highest photocurrent density value of -4.04 mA/cm2 was obtained for the 30-wt% sample, which had the lowest Cu2O (111)/ ZnO (101) XRD peak intensity ratio. The highest photocurrent density value from the 30-wt% sample was approximately 2.35 times higher than that from the non-composite Cu2O film (0-wt% sample). From this study, we found that adding Zn could improve the photocurrent values of Zn-Cu2O composite films.

  5. TiO2 membranes for concurrent photocatalytic organic degradation and corrosion protection

    NASA Astrophysics Data System (ADS)

    Liang, Robert; Hatat-Fraile, Melisa; He, Horatio; Arlos, Maricor; Servos, Mark R.; Zhou, Y. Norman

    2015-10-01

    Organic contaminants and corrosion in water treatment effluents are a current global problem and the development of effective methods to facilitate the removal of organic contaminants and corrosion control strategies are required to mitigate this problem. TiO2 nanomaterials that are exposed to UV light can generate electron-hole pairs, which undergo redox reactions to produce hydroxyl radicals from adsorbed molecular oxygen. They hydroxyl radicals are able to oxidize organic contaminants in water. This same process can be used in conjunction to protect metals from corrosion via cathodic polarization. In this work, TiO2 nanomaterials were synthesized and electrophoretically deposited on conductive substrates to serve as films or membranes. An illuminated TiO2 film on a conductive surface served as the photoanode and assisted in the cathodic protection of stainless steel (SS304) and the degradation of organic pollutants, in this case glucose. This proof-of-concept relied on photoelectrochemical experiments conducted using a potentiostat and a xenon lamp illumination source. The open-circuit potential changes that determine whether a metal is protected from corrosion under illumination was observed; and the electrical characteristics of the TiO2 film or membrane under dark and arc lamp illumination conditions were also analyzed. Furthermore, the effect of organic contaminants on the photocathodic protection mechanism and the oxidation of glucose during this process were explored.

  6. Spatiotemporal norepinephrine mapping using a high-density CMOS microelectrode array.

    PubMed

    Wydallis, John B; Feeny, Rachel M; Wilson, William; Kern, Tucker; Chen, Tom; Tobet, Stuart; Reynolds, Melissa M; Henry, Charles S

    2015-10-21

    A high-density amperometric electrode array containing 8192 individually addressable platinum working electrodes with an integrated potentiostat fabricated using Complementary Metal Oxide Semiconductor (CMOS) processes is reported. The array was designed to enable electrochemical imaging of chemical gradients with high spatiotemporal resolution. Electrodes are arranged over a 2 mm × 2 mm surface area into 64 subarrays consisting of 128 individual Pt working electrodes as well as Pt pseudo-reference and auxiliary electrodes. Amperometric measurements of norepinephrine in tissue culture media were used to demonstrate the ability of the array to measure concentration gradients in complex media. Poly(dimethylsiloxane) microfluidics were incorporated to control the chemical concentrations in time and space, and the electrochemical response at each electrode was monitored to generate electrochemical heat maps, demonstrating the array's imaging capabilities. A temporal resolution of 10 ms can be achieved by simultaneously monitoring a single subarray of 128 electrodes. The entire 2 mm × 2 mm area can be electrochemically imaged in 64 seconds by cycling through all subarrays at a rate of 1 Hz per subarray. Monitoring diffusional transport of norepinephrine is used to demonstrate the spatiotemporal resolution capabilities of the system. PMID:26333296

  7. Characterization of YSZ solid oxide fuel cells electrolyte deposited by atmospheric plasma spraying and low pressure plasma spraying

    NASA Astrophysics Data System (ADS)

    Zhang, C.; Liao, H. L.; Li, W. Y.; Zhang, G.; Coddet, C.; Zhang, C.; Li, C. J.; Li, C. X.; Ning, X. J.

    2006-12-01

    Yttria doped zirconia has been widely used as electrolyte materials for solid oxide fuel cells (SOFC). Plasma spraying is a cost-effective process to deposit YSZ electrolyte. In this study, the 8 mol% Y2O3 stabilized ZrO2 (YSZ) layer was deposited by low pressure plasma spraying (LPPS) and atmospheric plasma spraying (APS) with fused-crushed and agglomerated powders to examine the effect of spray method and particle size on the electrical conductivity and gas permeability of YSZ coating. The microstructure of YSZ coating was characterized by scanning electron microscopy and x-ray diffraction analysis. The results showed that the gas permeability was significantly influenced by powder structure. The gas permeability of YSZ coating deposited by fused-crushed powder is one order lower in magnitude than that by agglomerated powder. Moreover, the gas permeability of YSZ deposited by LPPS is lower than that of APS YSZ. The electrical conductivity of the deposits through thickness direction was measured by potentiostat/galvanostat based on three-electrode assembly approach. The electrical conductivity of YSZ coating deposited by low pressure plasma spraying with fused-crushed powder of small particle size was 0.043 S cm-1 at 100 °C, which is about 20% higher than that of atmospheric plasma spraying YSZ with the same powder.

  8. Energy-efficient treatment of organic wastewater streams using a rotatable bioelectrochemical contactor (RBEC).

    PubMed

    Cheng, Ka Yu; Ho, Goen; Cord-Ruwisch, Ralf

    2012-12-01

    A membraneless bioelectrochemical system - rotatable bio-electrochemical contactor (RBEC) consists of an array of rotatable electrode disks was developed to convert the chemical energy from wastewater organics (acetate) directly into electricity. Each rotatable electrode disk had an upper-air exposing and a lower-water submerging halves. Intermittent rotation (180°) enabled each halve to alternately serve as anode and cathode. Removal of chemical oxygen demand (COD) was increased by 15% (from 0.79 to 0.91 kg COD m(-3) d(-1)) by allowing electron flow from the lower to the upper disk halves. Coupling with a potentiostat could alleviate cathodic limitation and increased COD removal to 1.32 kg COD m(-3) day(-1) (HRT 5h). About 40% of the COD removed was via current, indicating that the biofilm could use the lower half disk as electron acceptor. The RBEC removed COD more energy-efficiently than conventional activated sludge processes as active aeration is not required (0.47 vs. 0.7-2.0 kW h kg COD(-1)). PMID:22209129

  9. Design of a high-speed electrochemical scanning tunneling microscope

    NASA Astrophysics Data System (ADS)

    Yanson, Y. I.; Schenkel, F.; Rost, M. J.

    2013-02-01

    In this paper, we present a bottom-up approach to designing and constructing a high-speed electrochemical scanning tunneling microscope (EC-STM). Using finite element analysis (FEA) calculations of the frequency response of the whole mechanical loop of the STM, we analyzed several geometries to find the most stable one that could facilitate fast scanning. To test the FEA results, we conducted measurements of the vibration amplitudes using a prototype STM setup. Based on the FEA analysis and the measurement results, we identified the potentially most disturbing vibration modes that could impair fast scanning. By modifying the design of some parts of the EC-STM, we reduced the amplitudes as well as increased the resonance frequencies of these modes. Additionally, we designed and constructed an electrochemical flow-cell that allows STM imaging in a flowing electrolyte, and built a bi-potentiostat to achieve electrochemical potential control during the measurements. Finally, we present STM images acquired during high-speed imaging in air as well as in an electrochemical environment using our newly-developed EC-STM.

  10. Analytical detection of biological thiols in a microchip capillary channel.

    PubMed

    Chand, Rohit; Jha, Sandeep Kumar; Islam, Kamrul; Han, Dawoon; Shin, Ik-Soo; Kim, Yong-Sang

    2013-02-15

    Sulfur-containing amino acids, such as cysteine and homocysteine play crucial roles in biological systems for the diagnosis of medical states. In this regard, this paper deals with separation, aliquot and detection of amino thiols on a microchip capillary electrophoresis with electrochemical detection in an inverted double Y-shaped microchannel. Unlike the conventional capillary electrophoresis, the modified microchannel design helps in storing the separated thiols in different reservoirs for further analysis, if required; and also eliminates the need of electrodes regeneration. The device was fabricated using conventional photolithographic technique which consisted of gold microelectrodes on a soda lime glass wafer and microchannels in PDMS mold. Multiple detections were performed using in-house fabricated dual potentiostat. Based on amperometric detection, cysteine and homocysteine were analyzed in 105 s and 120 s, respectively after diverting in branched channels. Repeated experiments proved the good reproducibility of the device. The device produced a linear response for both cysteine and homocysteine in electrochemical analysis. To prove the practicality of device, we also analyzed cysteine and homocysteine in real blood samples without any pre-treatment. Upon calculation, the device showed a very low limit of detection of 0.05 μM. The modified microchip design shall find a broad range of analytical applications involving assays of thiols and other biological compounds. PMID:22940195

  11. Electrochromic properties of nano-structured nickel oxide thin film prepared by spray pyrolysis method

    NASA Astrophysics Data System (ADS)

    Lin, Sheng-Hui; Chen, Fu-Rong; Kai, Ji-Jung

    2008-01-01

    In this study, we present a simple method to improve the electrochromic properties of a nickel oxide thin film. The method involves a three-step process—(a) conducting indium tin oxide (ITO) nano-particles were first sprayed onto a conducting substrate to form a porous nano-structured ITO layer, (b) nickel oxide film was then deposited onto the nano-structured ITO layer by a spray pyrolysis technique, and (c) the substrate, ITO nano-particles layer and nickel oxide film were annealed at high temperature of 300 °C to improve adhesion of these three layers. The microstructure of the resulting electrochromic cell was investigated using scanning electron microscopy. It is evident that the nickel oxide film covers the surface of the ITO nano-particle layer and forms a nano-structured nickel oxide (NSNO) film. The switching time and contrast were characterized by Autolab PGSTAT12 potentiostat and Jasco V-570 spectrophotometer. The results suggest that the transmittance contrast and switching time of NSNO are slightly superior to those of a conventional nickel oxide (CNO) film. However, the cycling durability of NSNO can be much better than that of CNO.

  12. Design and applications of an in situ electrochemical NMR cell

    NASA Astrophysics Data System (ADS)

    Zhang, Xiaocan; Zwanziger, Josef W.

    2011-01-01

    A device using a three-electrode electrochemical cell (referred to as an ECNMR cell) was successfully constructed that could be used in a standard 5 mm NMR probe to acquire high-resolution NMR spectra while the working electrode was held at a constant electrical potential. The working electrode was a 20 nm thick gold film thermally coated on the outside of an inner 3 mm glass tube. An underlayer consisting of (3-mercaptopropyl)trimethoxy-silane was coated on the glass surface in order to improve its adhesion to gold. Tests showed prolonged life of the gold film. Details of the design and construction of the ECNMR cell are described. The ECNMR cell could be routinely used in a multi-user service high-resolution NMR instrument under oxygen-free conditions in both aqueous and non-aqueous solvents. Different approaches were applied to suppress the noise transmitted between the potentiostat and the NMR spectrometer. These approaches were shown to be effective in reducing background noise in the NMR spectra. The electrochemical and NMR performance of the ECNMR cell is presented. The reduction of 1,4-benzoquinone in both aqueous and non-aqueous solvents was used for testing. The evolution of the in situ ECNMR spectra with time demonstrated that use of the ECNMR cell was feasible. Studies of caffeic acid and 9-chloroanthracene using this ECNMR cell were undertaken to explore its applications, such as monitoring reactions and studying their reaction mechanisms.

  13. Integrated circuit-based electrochemical sensor for spatially resolved detection of redox-active metabolites in biofilms.

    PubMed

    Bellin, Daniel L; Sakhtah, Hassan; Rosenstein, Jacob K; Levine, Peter M; Thimot, Jordan; Emmett, Kevin; Dietrich, Lars E P; Shepard, Kenneth L

    2014-01-01

    Despite advances in monitoring spatiotemporal expression patterns of genes and proteins with fluorescent probes, direct detection of metabolites and small molecules remains challenging. A technique for spatially resolved detection of small molecules would benefit the study of redox-active metabolites that are produced by microbial biofilms and can affect their development. Here we present an integrated circuit-based electrochemical sensing platform featuring an array of working electrodes and parallel potentiostat channels. 'Images' over a 3.25 × 0.9 mm(2) area can be captured with a diffusion-limited spatial resolution of 750 μm. We demonstrate that square wave voltammetry can be used to detect, identify and quantify (for concentrations as low as 2.6 μM) four distinct redox-active metabolites called phenazines. We characterize phenazine production in both wild-type and mutant Pseudomonas aeruginosa PA14 colony biofilms, and find correlations with fluorescent reporter imaging of phenazine biosynthetic gene expression. PMID:24510163

  14. Compact Electrochemical System Using On-Chip Sensor Electrodes and Integrated Devices

    NASA Astrophysics Data System (ADS)

    Yamazaki, Tomoyuki; Ikeda, Takaaki; Ishida, Makoto; Sawada, Kazuaki

    2011-04-01

    We report a compact electrochemical sensing system to implement cyclic voltammetry. This type of sensor needs a working electrode, counter electrode, and reference electrode, all of which were integrated on a single chip. The electrochemical system also needs a potentiostat and an input voltage-generating circuit, which were developed using on-chip active devices and a few discrete passive components. This is the first sensor system incorporating electrode-side input voltage generation for electrochemical measurements using an on-chip operational amplifier, which replaces a bulky external voltage controller. A continuous cyclic voltammetry measurement was conducted with a well-studied ferricyanide solution to demonstrate the operation of the intelligent sensor chip. A clear peak was observed and linearity to the target chemical concentration was obtained between the peak height and concentration of the ferricyanide solution. With potential for mass production and small size, this sensor chip could be the best candidate to realize point-of-care testing. This sensor chip is a milestone of a fully integrated electrochemical sensor chip.

  15. Assessment of corrosion rate in prestressed concrete with acoustic emission

    NASA Astrophysics Data System (ADS)

    Mangual, Jesé; ElBatanouny, Mohamed K.; Vélez, William; Ziehl, Paul; Matta, Fabio; González, Miguel

    2011-04-01

    Acoustic Emission (AE) sensing was employed to assess the rate of corrosion of steel strands in small scale concrete block specimens. The corrosion process was accelerated in a laboratory environment using a potentiostat to supply a constant potential difference with a 3% NaCl solution as the electrolyte. The embedded prestressing steel strand served as the anode, and a copper plate served as the cathode. Corrosion rate, half-cell potential measurements, and AE activity were recorded continuously throughout each test and examined to assess the development of corrosion and its rate. At the end of each test the steel strands were cleaned and re-weighed to determine the mass loss and evaluate it vis-á-vis the AE data. The initiation and propagation phases of corrosion were correlated with the percentage mass loss of steel and the acquired AE signals. Results indicate that AE monitoring may be a useful aid in the detection and differentiation of the steel deterioration phases, and estimation of the locations of corroded areas.

  16. A new method for determining the acid number of biodiesel based on coulometric titration.

    PubMed

    Barbieri Gonzaga, Fabiano; Pereira Sobral, Sidney

    2012-08-15

    A new method is proposed for determining the acid number (AN) of biodiesel using coulometric titration with potentiometric detection, basically employing a potentiostat/galvanostat and an electrochemical cell containing a platinum electrode, a silver electrode, and a combination pH electrode. The method involves a sequential application of a constant current between the platinum (cathode) and silver (anode) electrodes, followed by measuring the potential of the combination pH electrode, using an isopropanol/water mixture as solvent and LiCl as the supporting electrolyte. A preliminary evaluation of the new method, using acetic acid for doping a biodiesel sample, showed an average recovery of 100.1%. Compared to a volumetric titration-based method for determining the AN of several biodiesel samples (ranging from about 0.18 to 0.95 mg g(-1)), the new method produced statistically similar results with better repeatability. Compared to other works reported in the literature, the new method presented an average repeatability up to 3.2 times better and employed a sample size up to 20 times smaller. PMID:22841067

  17. Virtual electrochemical nitric oxide analyzer using copper, zinc superoxide dismutase immobilized on carbon nanotubes in polypyrrole matrix.

    TOXLINE Toxicology Bibliographic Information

    Madasamy T; Pandiaraj M; Balamurugan M; Karnewar S; Benjamin AR; Venkatesh KA; Vairamani K; Kotamraju S; Karunakaran C

    2012-10-15

    In this work, we have designed and developed a novel and cost effective virtual electrochemical analyzer for the measurement of NO in exhaled breath and from hydrogen peroxide stimulated endothelial cells using home-made potentiostat. Here, data acquisition system (NI MyDAQ) was used to acquire the data from the electrochemical oxidation of NO mediated by copper, zinc superoxide dismutase (Cu,ZnSOD). The electrochemical control programs (graphical user-interface software) were developed using LabVIEW 10.0 to sweep the potential, acquire the current response and process the acquired current signal. The Cu,ZnSOD (SOD1) immobilized on the carbon nanotubes in polypyrrole modified platinum electrode was used as the NO biosensor. The electrochemical behavior of the SOD1 modified electrode exhibited the characteristic quasi-reversible redox peak at the potential, +0.06 V vs. Ag/AgCl. The biological interferences were eliminated by nafion coated SOD1 electrode and then NO was measured selectively. Further, this biosensor showed a wide linear range of response over the concentration of NO from 0.1 μM to 1 mM with a detection limit of 0.1 μM and high sensitivity of 1.1 μA μM(-1). The electroanalytical results obtained here using the developed virtual electrochemical instrument were also compared with the standard cyclic voltammetry instrument and found in agreement with each other.

  18. Microchip electrophoresis with amperometric detection for the study of the generation of nitric oxide by NONOate salts

    PubMed Central

    Gunasekara, Dulan B.; Hulvey, Matthew K.; Lunte, Susan M.; da Silva, José Alberto Fracassi

    2013-01-01

    Microchip electrophoresis (ME) with electrochemical detection was used to monitor nitric oxide (NO) production from diethylammonium (Z)-1-(N,N-diethylamino)diazen-1-ium-1,2-diolate (DEA/NO) and 1-(hydroxyl-NNO-azoxy)-L-proline disodium salt (PROLI/NO). NO was generated through acid hydrolysis of these NONOate salts. The products of acid hydrolysis were introduced into a 5-cm separation channel using gated injection. The separation was accomplished using reverse polarity and a background electrolyte consisting of 10 mM boric acid and 2 mM tetradecyltrimethylammonium bromide, pH 11. Electrochemical detection was performed using an isolated potentiostat in an in-channel configuration. Potentials applied to the working electrode, typically higher than +1.0 V vs. Ag/AgCl, allowed the direct detection of nitrite, NO, DEA/NO, and PROLI/NO. Baseline resolution was achieved for the separation of PROLI/NO and NO while resolution between DEA/NO and NO was poor (1.0±0.2). Nitrite was present in all samples tested. PMID:22415023

  19. LabVIEW-based sequential-injection analysis system for the determination of trace metals by square-wave anodic and adsorptive stripping voltammetry on mercury-film electrodes.

    PubMed

    Economou, Anastasios; Voulgaropoulos, Anastasios

    2003-01-01

    The development of a dedicated automated sequential-injection analysis apparatus for anodic stripping voltammetry (ASV) and adsorptive stripping voltammetry (AdSV) is reported. The instrument comprised a peristaltic pump, a multiposition selector valve and a home-made potentiostat and used a mercury-film electrode as the working electrodes in a thin-layer electrochemical detector. Programming of the experimental sequence was performed in LabVIEW 5.1. The sequence of operations included formation of the mercury film, electrolytic or adsorptive accumulation of the analyte on the electrode surface, recording of the voltammetric current-potential response, and cleaning of the electrode. The stripping step was carried out by applying a square-wave (SW) potential-time excitation signal to the working electrode. The instrument allowed unattended operation since multiple-step sequences could be readily implemented through the purpose-built software. The utility of the analyser was tested for the determination of copper(II), cadmium(II), lead(II) and zinc(II) by SWASV and of nickel(II), cobalt(II) and uranium(VI) by SWAdSV. PMID:18924623

  20. Electrochemical Oscillations of Nickel Electrodissolution in an Epoxy-Based Microchip Flow Cell

    PubMed Central

    Cioffi, Alexander G.; Martin, R. Scott; Kiss, István Z.

    2011-01-01

    We investigate the nonlinear dynamics of transpassive electrodissolution of nickel in sulfuric acid in an epoxy-based microchip flow cell. We observed bistability, smooth, relaxation, and period-2 waveform current oscillations with external resistance attached to the electrode in the microfabricated electrochemical cell with 0.05 mm diameter Ni wire under potentiostatic control. Experiments with 1mm × 0.1 mm Ni electrode show spontaneous oscillations without attached external resistance; similar surface area electrode in macrocell does not exhibit spontaneous oscillations. Combined experimental and numerical studies show that spontaneous oscillation with the on-chip fabricated electrochemical cell occurs because of the unusually large ohmic potential drop due to the constrained current in the narrow flow channel. This large IR potential drop is expected to have an important role in destabilizing negative differential resistance electrochemical (e.g., metal dissolution and electrocatalytic) systems in on-chip integrated microfludic flow cells. The proposed experimental setup can be extendend to multi-electrode configurations; the epoxy-based substrate procedure thus holds promise in electroanalytical applications that require collector-generator multi-electrodes wires with various electrode sizes, compositions, and spacings as well as controlled flow conditions. PMID:21822407

  1. A liquid-junction-free reference electrode based on a PEDOT solid-contact and ionogel capping membrane.

    PubMed

    Zuliani, Claudio; Matzeu, Giusy; Diamond, Dermot

    2014-07-01

    Liquid-junction-free reference electrodes have been prepared on screen printed substrates using poly-3,4-ethylenedioxythiophene (PEDOT) as solid-contact and novel ionogels as capping membrane. The chemico-physical properties of the PEDOT layer were tuned by changing the electropolymerization media and the electrodeposition technique. Electrodepositing PEDOT films potentiostatically or potentiodynamically were found to have a significant impact on the stability of the electrodes during the conditioning step. Optimization of the capping membrane formulation, e.g., acrylate monomers, ionic liquid, cross-linkers and photo-initiators, produced electrodes with properties almost equivalent with a commercial reference electrode. Thus, calibration plots of Na(+) ion-selective electrodes against the optimized solid-contact ionogel reference electrodes (SCI-REs) or against a double-liquid junction Ag/AgCl electrode did not present any significant difference. Such SCI-REs may provide an effective route to the generation of future low-cost components for potentiometric sensing strips. PMID:24840415

  2. Ultrafast charge separation dynamics in opaque, operational dye-sensitized solar cells revealed by femtosecond diffuse reflectance spectroscopy

    PubMed Central

    Ghadiri, Elham; Zakeeruddin, Shaik M.; Hagfeldt, Anders; Grätzel, Michael; Moser, Jacques-E.

    2016-01-01

    Efficient dye-sensitized solar cells are based on highly diffusive mesoscopic layers that render these devices opaque and unsuitable for ultrafast transient absorption spectroscopy measurements in transmission mode. We developed a novel sub-200 femtosecond time-resolved diffuse reflectance spectroscopy scheme combined with potentiostatic control to study various solar cells in fully operational condition. We studied performance optimized devices based on liquid redox electrolytes and opaque TiO2 films, as well as other morphologies, such as TiO2 fibers and nanotubes. Charge injection from the Z907 dye in all TiO2 morphologies was observed to take place in the sub-200 fs time scale. The kinetics of electron-hole back recombination has features in the picosecond to nanosecond time scale. This observation is significantly different from what was reported in the literature where the electron-hole back recombination for transparent films of small particles is generally accepted to occur on a longer time scale of microseconds. The kinetics of the ultrafast electron injection remained unchanged for voltages between +500 mV and –690 mV, where the injection yield eventually drops steeply. The primary charge separation in Y123 organic dye based devices was clearly slower occurring in two picoseconds and no kinetic component on the shorter femtosecond time scale was recorded. PMID:27095505

  3. Ion transport in polycarbonate based solid polymer electrolytes: experimental and computational investigations.

    PubMed

    Sun, Bing; Mindemark, Jonas; V Morozov, Evgeny; Costa, Luciano T; Bergman, Martin; Johansson, Patrik; Fang, Yuan; Furó, István; Brandell, Daniel

    2016-03-30

    Among the alternative host materials for solid polymer electrolytes (SPEs), polycarbonates have recently shown promising functionality in all-solid-state lithium batteries from ambient to elevated temperatures. While the computational and experimental investigations of ion conduction in conventional polyethers have been extensive, the ion transport in polycarbonates has been much less studied. The present work investigates the ionic transport behavior in SPEs based on poly(trimethylene carbonate) (PTMC) and its co-polymer with ε-caprolactone (CL) via both experimental and computational approaches. FTIR spectra indicated a preferential local coordination between Li(+) and ester carbonyl oxygen atoms in the P(TMC20CL80) co-polymer SPE. Diffusion NMR revealed that the co-polymer SPE also displays higher ion mobilities than PTMC. For both systems, locally oriented polymer domains, a few hundred nanometers in size and with limited connections between them, were inferred from the NMR spin relaxation and diffusion data. Potentiostatic polarization experiments revealed notably higher cationic transference numbers in the polycarbonate based SPEs as compared to conventional polyether based SPEs. In addition, MD simulations provided atomic-scale insight into the structure-dynamics properties, including confirmation of a preferential Li(+)-carbonyl oxygen atom coordination, with a preference in coordination to the ester based monomers. A coupling of the Li-ion dynamics to the polymer chain dynamics was indicated by both simulations and experiments. PMID:26984668

  4. Reduction mechanism of sulfur in lithium-sulfur battery: From elemental sulfur to polysulfide

    SciTech Connect

    Zheng, Dong; Yang, Xuran; Zhang, Xiaoqing; Wang, Jiankun; Qu, Deyu; Qu, Deyang

    2015-10-30

    In this study, the polysulfide ions formed during the first reduction wave of sulfur in Li–S battery were determined through both in-situ and ex-situ derivatization of polysulfides. By comparing the cyclic voltammetric results with and without the derivatization reagent (methyl triflate) as well as the in-situ and ex-situ derivatization results under potentiostatic condition, in-situ derivatization was found to be more appropriate than its ex-situ counterpart, since subsequent fast chemical reactions between the polysulfides and sulfur may occur during the timeframe of ex-situ procedures. It was found that the major polysulfide ions formed at the first reduction wave of elemental sulfur were the S42– and S52– species, while the widely accepted reduction products of S82– and S62– for the first reduction wave were in low abundance.

  5. Pulse electrodeposition of adherent nickel coatings onto anodized aluminium surfaces

    NASA Astrophysics Data System (ADS)

    Frantz, Cédric; Vichery, Charlotte; Zechner, Johannes; Frey, Damian; Bürki, Gerhard; Cebeci, Halil; Michler, Johann; Philippe, Laetitia

    2015-03-01

    Aluminium is one of the mostly used elements in the industry because of its abundance and low weight. However, the deposition of a metallic coating requires performing the so-called zincate pre-treatment in order to allow the formation of inter-metallic bonds and thereby achieving sufficient adherence. In this work, porous anodic aluminium oxide (AAO) is used as an anchoring intermediate layer for nickel coatings. AAO is grown anodically in sulfuric acid and nickel coatings are deposited by potentiostatic reverse pulse electrodeposition onto as-anodized aluminium surfaces. The electrodeposition of nickel is initiated onto the electrochemically thinned barrier layer of AAO and pursued until the complete covering of the oxide. The electrochemical behavior of Watts and sulfamate baths is investigated by cyclic voltammetry for different barrier layer thickness, allowing to validate the thinning conditions and to determine the appropriate deposition potential of nickel. GD-OES measurements show that low duty cycles are necessary to achieve high filling ratio of the AAO. SEM micrographs show that a smooth uniform coating is obtained when nickel is deposited in presence of additives.

  6. Applications of Planar ITO Electrodes for Studying of Some Biochemical Activities

    NASA Astrophysics Data System (ADS)

    Learngarunsri, P.; Chaiyen, P.; Srikhirin, T.; Veerasai, W.; Dangtip, S.

    Trends in disposable and handheld biosensors have called for miniaturized and planar electrodes in the place of conventional bulky ones. In this work, thin tin-doped indium oxide (ITO) film coated on glass were used as a based electrode in a three-electrode electrochemical system to follow some biochemical activities, such as NADH and phenol activity. The reference electrode is made on ITO layer by electro-deposition of thin nickel layer and silver layer, consecutively, followed by chlorination of silver surface by electrochemical potentiostatic method. The plain planar ITO-coated glasses were used as both counter electrode and working electrodes. Cyclic-voltammetry measurements; which follow an oxidation of 200 μM nicotinamide adenine dinucleotide (NADH) in 0.1 M KCl, show current peak of 8.5 μA. Another case was also to follow the NADH oxidation but in competition with its coupling activity with flavin mononucleotide (FMN). In this case, cyclic-voltammetry measurements were carried out of 200 μM NADH in 50 mM sodium phosphate; current peak of 1.3 μA was observed.

  7. Role of surfactant-mediated electrodeposited titanium oxide substrate in improving electrocatalytic features of supported platinum particles

    NASA Astrophysics Data System (ADS)

    Spătaru, Tanţa; Preda, Loredana; Osiceanu, Petre; Munteanu, Cornel; Anastasescu, Mihai; Marcu, Maria; Spătaru, Nicolae

    2014-01-01

    A new hybrid system with improved photocatalytic and electrocatalytic performances was obtained by two-step potentiostatic deposition on highly boron-doped diamond (BDD) substrate. First, hydrated TiO2 was anodically deposited from a TiCl3 aqueous solution, both in the presence and in the absence of sodium dodecyl sulfate (SDS). The study of the UV irradiation effect evidenced that titanium oxide coatings obtained by surfactant-assisted electrodeposition (TiO2:SDS) exhibit enhanced photocurrent, due to its very rough texture and presumably to better efficiency of charge carrier separation. Electrochemical deposition of platinum on the oxide-coated BDD was carried out in a second step and AFM, SEM and XPS measurements have shown that, on the TiO2:SDS substrate, Pt particles are smaller, more uniformly distributed, and tend to form clusters, leading to a specific surface area of the electrocatalyst of ca. 6.55 m2 g-1. Carbon monoxide stripping experiments demonstrated that, when deposited on TiO2:SDS, Pt particles are also less sensitive to CO-poisoning during methanol anodic oxidation.

  8. Facile synthesis of polypyrrole functionalized nickel foam with catalytic activity comparable to Pt for the poly-generation of hydrogen and electricity

    NASA Astrophysics Data System (ADS)

    Tang, Tiantian; Li, Kan; Shen, Zhemin; Sun, Tonghua; Wang, Yalin; Jia, Jinping

    2016-01-01

    Polypyrrole functionalized nickel foam is facilely prepared through the potentiostatic electrodeposition. The PPy-functionalized Ni foam functions as a hydrogen-evolution cathode in a rotating disk photocatalytic fuel cell, in which hydrogen energy and electric power are generated by consuming organic wastes. The PPy-functionalized Ni foam cathode exhibits stable catalytic activities after thirteen continuous runs. Compared with net or plate structure, the Ni foam with a unique three-dimensional reticulate structure is conducive to the electrodeposition of PPy. Compared with Pt-group electrode, PPy-coated Ni foam shows a satisfactory catalytic performance for the H2 evolution. The combination of PPy and Ni forms a synergistic effect for the rapid trapping and removal of proton from solution and the catalytic reduction of proton to hydrogen. The PPy-functionalized Ni foam could be applied in photocatalytic and photoelectrochemical generation of H2. In all, we report a low cost, high efficient and earth abundant PPy-functionalized Ni foam with a satisfactory catalytic activities comparable to Pt for the practical application of poly-generation of hydrogen and electricity.

  9. Potential COntrol Under Thin Aqueous Layers Using a Kelvin Probe

    SciTech Connect

    G.S. Frankel; B. Maier; M. Stratman; M. Rohwerder; A. Michalik; J. Dora; M. Wicinski

    2006-08-17

    Kelvin Probes can be modified to control as well as monitor potential. The design and operation of two different Kelvin Probe Potentiostats (KPPs) are described in this paper. One approach uses a permanent magnet and double coil to oscillate the needle at a fixed frequency, an AC backing potential, and software analysis and control schemes. This technique can also control the distance between the tip and sample, thereby tracking the topography of the sample. Both KPPs were used to make measurements on Type 304L stainless steel under thin layers of electrolyte. Cathodic polarization curves exhibited a limiting current density associated with oxygen reduction. The limiting current density varied with solution layer thickness over a finite range of thickness. Anodic polarization curves on 304L in a thin layer of chloride solution resulted in pitting corrosion. The breakdown potential did not vary with solution layer thickness. However, the thin layer was observed to increase in volume remarkably during pit growth owing to the absorption of water from the high humidity environment into the layer with ionic strength increased by the pit dissolution. The open circuit potential (OCP) and solution layer thickness were monitored during drying out of a thin electrolyte layer. Pitting corrosion initiated, as indicated by a sharp drop in the OCP, as the solution thinned and increased in concentration.

  10. Comparison of Pt and Pd catalysts for hydrogen pump separation from reformate

    NASA Astrophysics Data System (ADS)

    Wu, Xuemei; Benziger, Jay; He, Gaohong

    2012-11-01

    Hydrogen recovery from CO2/H2 reformate mixtures by selective electrochemical pumping was compared from carbon supported Pt and Pd catalysts. Catalyst coated membranes were prepared by air-brushing a suspension of commercially available 20 wt% Pt/C or 20 wt% Pd/C catalysts and solubilized Nafion in methanol onto Nafion 115 membranes. Electrochemical activity and separation efficiency for the different catalyst layer formulations were evaluated by cyclic voltammetry, polarization and potentiostatic hydrogen pumping. The effective membrane-electrode-assembly (MEA) resistance increased due to dilution of H2 by CO2; the effective MEA resistance was greater for Pd/C catalysts than for Pt/C catalysts. CO2 adsorbed more strongly to Pd catalysts than Pt catalysts reducing the electrochemical active surface area available for hydrogen oxidation/reduction. Pd/C catalysts had an energy efficiency for hydrogen recovery from reformate mixtures approximately 80% that of Pt catalysts. Because Pd is ten times less costly than Pt the results presented here suggest that Pd/C catalysts would be a promising candidate for hydrogen pumps to recover H2 from reformate mixtures.

  11. Delayed feedback induced multirhythmicity in the oscillatory electrodissolution of copper.

    PubMed

    Nagy, Timea; Verner, Erika; Gáspár, Vilmos; Kori, Hiroshi; Kiss, István Z

    2015-06-01

    Occurrence of bi- and trirhythmicities (coexistence of two or three stable limit cycles, respectively, with distinctly different periods) has been studied experimentally by applying delayed feedback control to the copper-phosphoric acid electrochemical system oscillating close to a Hopf bifurcation point under potentiostatic condition. The oscillating electrode potential is delayed by τ and the difference between the present and delayed values is fed back to the circuit potential with a feedback gain K. The experiments were performed by determining the period of current oscillations T as a function of (both increasing and decreasing) τ at several fixed values of K. With small delay times, the period exhibits a sinusoidal type dependence on τ. However, with relatively large delays (typically τ ≫ T) for each feedback gain K, there exists a critical delay τcrit above which birhythmicity emerges. The experiments show that for weak feedback, Kτcrit is approximately constant. At very large delays, the dynamics becomes even more complex, and trirhythmicity could be observed. Results of numerical simulations based on a general kinetic model for metal electrodissolution were consistent with the experimental observations. The experimental and numerical results are also interpreted by using a phase model; the model parameters can be obtained from experimental data measured at small delay times. Analytical solutions to the phase model quantitatively predict the parameter regions for the appearance of birhythmicity in the experiments, and explain the almost constant value of Kτcrit for weak feedback. PMID:26117133

  12. Development of a commercial micro corrosion monitoring system

    NASA Astrophysics Data System (ADS)

    Niblock, Trevor G. E.; Surangalikar, Harshal S.; Morse, Jeffrey; Laskowski, Bernard C.; Castro-Cedeno, Mario H.; Wilson, Alan R.

    2002-11-01

    Analatom Inc. in conjunction with the DSTO (Defence Science & Technology Organisation) has been developing a micro Linear Polarization Resistance (LPR) system for assessing the integrity of high value structures. The device operates on the principle that as a metal corrodes, the oxide formed effectively creates an anodic cell. Hence, if the metal can be separated into two sections, a potential and resistance can be measured between each section. These values can be used to compute the effective mass loss of the device. By matching the material properties of the device with that of the structure whose "health" is being monitored, it is possible to establish a corrosion rate of the structure. Previous research at DSTO has shown that such a system can be fabricated and operated on the micro scale. The task has now been to develop the device into a commercially viable system; it is this development that is examined in this paper. In the original system, a potentiostat is used to evaluate the device for data relating the mass loss during corrosion. This system is now replaced with simplified electronics to reduce both the cost and size of the device. Signal conditioning into the LPR is critical as potentials over 20mV across the terminals can be a source of corrosion of the device. Micro controllers and small board computers are used to run this signal conditioning process and the LPR interface circuit.

  13. Phosphate Detection through a Cost-Effective Carbon Black Nanoparticle-Modified Screen-Printed Electrode Embedded in a Continuous Flow System.

    PubMed

    Talarico, Daria; Cinti, Stefano; Arduini, Fabiana; Amine, Aziz; Moscone, Danila; Palleschi, Giuseppe

    2015-07-01

    An automatable flow system for the continuous and long-term monitoring of the phosphate level has been developed using an amperometric detection method based on the use of a miniaturized sensor. This method is based on the monitoring of an electroactive complex obtained by the reaction between phosphate and molybdate that is consequently reduced at the electrode surface. The use of a screen-printed electrode modified with carbon black nanoparticles (CBNPs) leads to the quantification of the complex at low potential, because CBNPs are capable of electrocatalitically enhancing the phosphomolybdate complex reduction at +125 mV versus Ag/AgCl without fouling problems. The developed system also incorporates reagents and waste storage and is connected to a portable potentiostat for rapid detection and quantification of phosphate. Main analytical parameters, such as working potential, reagent concentration, type of cell, and flow rate, were evaluated and optimized. This system was characterized by a low detection limit (6 μM). Interference studies were carried out. Good recovery percentages comprised between 89 and 131.5% were achieved in different water sources, highlighting its suitability for field measurements. PMID:26066782

  14. Development of Amperometric Biosensors Based on Nanostructured Tyrosinase-Conducting Polymer Composite Electrodes

    PubMed Central

    Lupu, Stelian; Lete, Cecilia; Balaure, Paul Cătălin; Caval, Dan Ion; Mihailciuc, Constantin; Lakard, Boris; Hihn, Jean-Yves; del Campo, Francisco Javier

    2013-01-01

    Bio-composite coatings consisting of poly(3,4-ethylenedioxythiophene) (PEDOT) and tyrosinase (Ty) were successfully electrodeposited on conventional size gold (Au) disk electrodes and microelectrode arrays using sinusoidal voltages. Electrochemical polymerization of the corresponding monomer was carried out in the presence of various Ty amounts in aqueous buffered solutions. The bio-composite coatings prepared using sinusoidal voltages and potentiostatic electrodeposition methods were compared in terms of morphology, electrochemical properties, and biocatalytic activity towards various analytes. The amperometric biosensors were tested in dopamine (DA) and catechol (CT) electroanalysis in aqueous buffered solutions. The analytical performance of the developed biosensors was investigated in terms of linear response range, detection limit, sensitivity, and repeatability. A semi-quantitative multi-analyte procedure for simultaneous determination of DA and CT was developed. The amperometric biosensor prepared using sinusoidal voltages showed much better analytical performance. The Au disk biosensor obtained by 50 mV alternating voltage amplitude displayed a linear response for DA concentrations ranging from 10 to 300 μM, with a detection limit of 4.18 μM. PMID:23698270

  15. Effect of Fluoride on Nickel-Titanium and Stainless Steel Orthodontic Archwires: An In-Vitro Study

    PubMed Central

    Heravi, Farzin; Moayed, Mohamad Hadi; Mokhber, Nima

    2015-01-01

    Objectives: The commonly used Nickel-Titanium (NiTi) archwires in orthodontic treatment are often exposed to fluoride-containing mouthwashes. The aim of this in-vitro study was to evaluate and compare the corrosion resistance of three commercially available NiTi archwires exposed to 0.05 wt% and 0.2 wt% fluoride mouthwashes. Materials and Methods: Three different types of NiTi archwires, 0.016″ in diameter, from Dentaurum, Global, and GAC, and a stainless steel archwire from Dentaurum were examined to assess their corrosion resistance in Fusayama-Meyer artificial saliva and in two other artificial saliva containing 0.05 wt% and 0.2 wt% sodium fluoride (NaF). After the primary setup of wires, they were tested by potentiodynamic and potentiostatic polarization and corrosion potential/time analyses. Their surfaces were evaluated using a scanning electronic microscope (SEM). Results: The results showed that all the wires were passive in artificial saliva. In contrast, by adding fluoride ions to the solution, the decrease in the archwires’ corrosion resistance was in direct proportion to the increase in fluoride concentration. Conclusion: The NiTi wires experienced deterioration of their corrosion properties under the effect of fluoride but not as much as the stainless steel archwires. PMID:26005454

  16. Construction and application of an amperometric xanthine biosensor based on zinc oxide nanoparticles-polypyrrole composite film.

    PubMed

    Devi, Rooma; Thakur, Manish; Pundir, C S

    2011-04-15

    Zinc oxide nanoparticles (ZnO-NPs) were synthesized from zinc nitrate by simple and efficient method in aqueous media at 55°C without any requirement of calcinations step. A mixture of ZnO-NPs and pyrrole was eletropolymerized on Pt electrode to form a ZnO-NPs-polypyrrole (PPy) composite film. Xanthine oxidase (XOD) was immobilized onto this nanocomposite film through physiosorption. The ZnO-NPs/polypyrrole/Pt electrode was characterized by Fourier transform infrared (FTIR), cyclic voltammetry (CV), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electrochemical impedance spectroscopy (EIS) before and after immobilization of XOD. The XOD/ZnO-NPs-PPy/Pt electrode as working electrode, Ag/AgCl as reference electrode and Pt wire as auxiliary electrode were connected through a potentiostat to construct a xanthine biosensor. The biosensor exhibited optimum response within 5s at pH 7.0, 35°C and linearity from 0.8 μM to 40 μM for xanthine with a detection limit 0.8 μM (S/E=3). Michaelis Menten constant (K(m)) for xanthine oxidase was 13.51 μM and I(max) 0.071 μA. The biosensor measured xanthine in fish meat and lost 40% of its initial activity after its 200 uses over 100 days, when stored at 4°C. PMID:21324666

  17. Electrochemistry combined on-line with electrospray mass spectrometry

    SciTech Connect

    Zhou, F.; Berkel, G.J.V.

    1995-10-15

    In this paper a variety of methods to couple electrochemistry on-line with electrospray mass spectrometry (EC/ES-MS) are presented, and the fundamental and analytical utility of this hybrid technique is illustrated. The major problems encountered in coupling EC and ES-MS are discussed, and means to overcome them are presented. Three types of electrochemical flow cells, viz., a thin-layer electrode flow-by cell, a tubular electrode flow-through cell, and a porous electrode flow-through cell, are discussed in regard to their suitability for this coupling. Methods for coupling each of these electrochemical cells on-line with ES-MS, either floated at or decoupled from the ES high voltage and controlled by a constant current supply, a constant potential supply, or a potentiostat are presented. Three applications are used to illustrate the utility and versatility of the EC/ES-MS combination: (1) the ionization of neutral analytes (i.e., perylene) for detection by ES-MS, (2) the study of the products of electrode reactions (i.e., nickel(II) octaethylporphyrin oxidation products), including relatively short-lived products (i.e., {Beta}-carotene oxidation products), and (3) the enhanced determination of metals (i.e., elemental silver) achieved by coupling anodic stripping voltammetry on-line with ES-MS. 52 refs., 6 figs.

  18. Flow microcapillary plasma mass spectrometry-based investigation of new Al-Cr-Fe complex metallic alloy passivation.

    PubMed

    Ott, N; Beni, A; Ulrich, A; Ludwig, C; Schmutz, P

    2014-03-01

    Al-Cr-Fe complex metallic alloys are new intermetallic phases with low surface energy, low friction, and high corrosion resistance down to very low pH values (0-2). Flow microcapillary plasma mass spectrometry under potentiostatic control was used to characterize the dynamic aspect of passivation of an Al-Cr-Fe gamma phase in acidic electrolytes, allowing a better insight on the parameters inducing chemical stability at the oxyhydroxide-solution interface. In sulfuric acid pH 0, low element dissolution rates (in the µg cm(-2) range after 60 min) evidenced the passive state of the Al-Cr-Fe gamma phase with a preferential over-stoichiometric dissolution of Al and Fe cations. Longer air-aging was found to be beneficial for stabilizing the passive film. In chloride-containing electrolytes, ten times higher Al dissolution rates were detected at open-circuit potential (OCP), indicating that the spontaneously formed passive film becomes unstable. However, electrochemical polarization at low passive potentials induces electrical field generated oxide film modification, increasing chemical stability at the oxyhydroxide-solution interface. In the high potential passive region, localized attack is initiated with subsequent active metal dissolution. PMID:24468364

  19. Corrosion behaviour of magnesium alloys coated with TiN by cathodic arc deposition in NaCl and Na{sub 2}SO{sub 4} solutions

    SciTech Connect

    Altun, Hikmet Sinici, Hakan

    2008-03-15

    Magnesium-based light-metal alloys belong to a class of structural materials with increasing industrial attention. Magnesium alloys show the lowest density among the engineering metallic materials, low cost and large availability. However, the limitations according to mechanical strength and the low corrosion resistance restrict their practical application. In this study, TiN was coated on magnesium-based AZ91 magnesium-aluminium-zinc alloy using cathodic arc PVD process. The corrosion behaviours of uncoated and coated magnesium alloys in 1% NaCl, 3% NaCl and 3% Na{sub 2}SO{sub 4} solutions and the influence of the coatings on the corrosion behaviour of the substrate were investigated utilizing potentiodynamic polarization tests. A potentiostat for electrochemical corrosion tests, a cathodic arc physical vapour deposition coating system for coating processes, a scanning electron microscopy for surface examination and elemental analysis of the coatings were used in this study. It was determined that corrosion resistance of magnesium alloys can be increased with TiN coating on the alloys using cathodic arc PVD process.

  20. Study of the effect of temperature on Pt dissolution in polymer electrolyte membrane fuel cells via accelerated stress tests

    NASA Astrophysics Data System (ADS)

    Dhanushkodi, S. R.; Kundu, S.; Fowler, M. W.; Pritzker, M. D.

    2014-01-01

    Operation of polymer electrolyte membrane fuel cells (PEMFC) at higher cell temperatures accelerates Pt dissolution in the catalyst layer. In this study, a Pt dissolution accelerated stress testing protocol involving the application of a potentiostatic square-wave with 3 s at 0.6 V followed by 3 s at 1.0 V was developed to test fuel cell membrane electrode assemblies (MEAs). The use of this Pt dissolution protocol at three different temperatures (40 °C, 60 °C and 80 °C) was investigated for the same membrane electrode assembly composition. Impedance analysis of the membrane electrode assemblies showed an increase in polarization resistance during the course of the accelerated stress testing. Polarization analysis and electrochemical active surface area (ECSA) loss measurements revealed evidence of increased cathode catalyst layer (CCL) degradation due to Pt dissolution and deposition in the membrane as the cell temperature was raised. Scanning electron microscope (SEM) images confirmed the formation of Pt bands in the membrane. A diagnostic expression was developed to estimate kinetic losses due to oxygen reduction using the effective platinum surface area (EPSA) estimated from cyclic voltammograms. The results indicated that performance degradation occurred mainly due to Pt loss.