Search results for: electrochemical methods

Authors: Sara Kamalisiahroudi, Jun Huang, Zhe Li, Jianbo Zhang

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Two types of commercial cylindrical lithium ion batteries (Panasonic 3.4 Ah NCR-18650B and Samsung 2.9 Ah INR-18650), were investigated experimentally. The capacities of these samples were individually measured using constant current-constant voltage (CC-CV) method at different ambient temperatures (-10 ℃, 0 ℃, 25 ℃). Their internal resistance was determined by electrochemical impedance spectroscopy (EIS) and pulse discharge methods. The cells with different configurations of parallel connection NCR-NCR, INR-INR and NCR-INR were charged/discharged at the aforementioned ambient temperatures. The results showed that the difference of internal resistance between cells much more evident at low temperatures. Furthermore, the parallel connection of NCR-NCR exhibits the most uniform temperature distribution in cells at -10 ℃, this feature is quite favorable for the safety of the battery pack.

Keywords: batteries in parallel connection, internal resistance, low temperature, temperature difference, current distribution

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Authors: K. S. Ghosh, Sagnik Bose, Kapil Tripati

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Potentiodynamic polarization studies carried out on AA2024 and AA2014 Al-Cu-Mg alloys of various tempers in 3.5 wt. % NaCl and in 3.5 wt. % NaCl + 1.0 % H2O2 solution characteristic E-i curves. Corrosion potential (Ecorr) value has shifted towards more negative potential with the increase of artificial aging time. The Ecorr value for the alloy tempers has also shifted anodically in presence of H2O2 in 3.5 % NaCl solution. Further, passivity phenomenon has been observed in all the alloy tempers when tested in 3.5 wt. % NaCl solution at pH 12. Stress corrosion cracking (SCC) behaviour of friction stir weld (FSW) joint of AA2014 alloy has been studied bu slow strain rate test (SSRT) in 3.5 wt. % NaCl solution. Optical micrographs of the corroded surfaces of polarised samples showed general corrosion, extensive pitting and intergranular corrosion as well. Further, potentiodynamic cyclic polarization curves displayed wide hysteresis loop indicating that the alloy tempers are susceptible to pit growth damage. Attempts have been made to explain the variation of observed electrochemical and SCC behaviour of the alloy tempers and the electrolyte conditions with the help of microstructural features.

Keywords: AA 2014 and AA 2024 Al-C-Mg alloy, artificial ageing, potentiodynamic polarization, TEM micrographs, stress corrosion cracking (SCC)

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Authors: Jana Tchekalarova, Stela Georgieva, Petia Peneva, Petar Todorov

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In the present study, a series of bioconjugates of N-modified hemorphine analogs containing second pharmacophore cinnamic acids (CA) or caffeic (KA) were synthesized by a traditional solid-phase Fmoc chemistry method for peptide synthesis. Electrochemical and fluorimetrical analysis and in vivo anticonvulsant activity in mice were conducted on the compounds. The three CA acids (H4-CA, H5-CA, and H7-CA) and three KA acids (H4-KA, H5-KA, and H7-KA)-conjugated hemorphine derivatives showed dose-dependent anticonvulsant activity in the maximal electroshock test (MES) in mice. The KA-conjugated H5-KA derivate was the only compound that suppressed clonic seizures at the lowest dose of 0.5 µg/mouse in the scPTZ test. The activity against the psychomotor seizures in the 6-Hz test was detected only for the H4-CA (0.5 µg) and H4-KA (0.5 µg and 1 µg), respectively. The peptide derivates did not exhibit neurotoxicity in the rotarod test. Our findings suggest that conjugated CA and KA hemorphine peptides can be used as a background for developing hemorphin-related analogs with anticonvulsant activity. Acknowledgements: This study is funded by the European Union-NextGenerationEU, through the National Recovery and Resilience Plan of the Republic of Bulgaria, project № BG-RRP-2.004-0002, "BiOrgaMCT".

Keywords: hemorphins, caffeic/cinnamic acid, anticonvulsant activity, electrochemistry, fluorimetry

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Authors: Maryam Mirabediny, Tsz Tin Yu, Jun Sun, Matthew Lee, Denis M. O’Carroll, Michael J. Manefield, Björn Akermark, Biswanath Das, Naresh Kumar

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Branched perfluorooctane sulfonic acid (PFOS) is recognized as a threatening environmental pollutant due to its high persistence and bioaccumulation in various environmental matrices as well as for its toxic effects on humans and wildlife, even at very low concentrations. This study reports the first investigation of branched PFOS defluorination catalyzed by metal phthalocyanines. The reaction conditions were optimized using the different reductants and temperatures. Cobalt phthalocyanine, when combined with Ti citrate as a reducing agent, was able to defluorinate 10.9% of technical PFOS within 8 hours. In contrast, vitamin B12 only showed 2.4% defluorination during the same period under similar conditions. The defluorination mediated by cobalt phthalocyanine and Ti citrate system corresponds to 54.5% of all branched PFOS isomers (br-PFOS isomers). Isomer-specific degradation was also investigated via high-resolution LC-orbitrap, followed by their relative rates. The difference in catalytic efficacy of various phthalocyanine complexes is rationalized by their structures and electrochemical response. Lastly, a new defluorination mechanism is proposed based on the newly detected degradation products after the phthalocyanines treatment and the previous studies.

Keywords: branched isomers, catalyst, reductive defluorination, water remediation

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Authors: Sudeshna Chandra, Christian Gäbler, Christian Schliebe, Heinrich Lang

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Highly branched dendrimers provide structural homogeneity, controlled composition, comparable size to biomolecules, internal porosity and multiple functional groups for conjugating reactions. Electro-active dendrimers containing multiple redox units have generated great interest in their use as electrode modifiers for development of biosensors. The electron transfer between the redox-active dendrimers and the biomolecules play a key role in developing a biosensor. Ferrocenes have multiple and electrochemically equivalent redox units that can act as electron “pool” in a system. The ferrocenyl-terminated polyamidoamine dendrimer is capable of transferring multiple numbers of electrons under the same applied potential. Therefore, they can be used for dual purposes: one in building a film over the electrode for immunosensors and the other for immobilizing biomolecules for sensing. Electrochemical immunosensor, thus developed, exhibit fast and sensitive analysis, inexpensive and involve no prior sample pre-treatment. Electrochemical amperometric immunosensors are even more promising because they can achieve a very low detection limit with high sensitivity. Detection of the cancer biomarkers at an early stage can provide crucial information for foundational research of life science, clinical diagnosis and prevention of disease. Elevated concentration of biomarkers in body fluid is an early indication of some type of cancerous disease and among all the biomarkers, IgG is the most common and extensively used clinical cancer biomarkers. We present an IgG (=immunoglobulin) electrochemical immunosensor using a newly synthesized redox-active ferrocenyl dendrimer of generation 2 (G2Fc) as glassy carbon electrode material for immobilizing the antibody. The electrochemical performance of the modified electrodes was assessed in both aqueous and non-aqueous media using varying scan rates to elucidate the reaction mechanism. The potential shift was found to be higher in an aqueous electrolyte due to presence of more H-bond which reduced the electrostatic attraction within the amido groups of the dendrimers. The cyclic voltammetric studies of the G2Fc-modified GCE in 0.1 M PBS solution of pH 7.2 showed a pair of well-defined redox peaks. The peak current decreased significantly with the immobilization of the anti-goat IgG. After the immunosensor is blocked with BSA, a further decrease in the peak current was observed due to the attachment of the protein BSA to the immunosensor. A significant decrease in the current signal of the BSA/anti-IgG/G2Fc/GCE was observed upon immobilizing IgG which may be due to the formation of immune-conjugates that blocks the tunneling of mass and electron transfer. The current signal was found to be directly related to the amount of IgG captured on the electrode surface. With increase in the concentration of IgG, there is a formation of an increasing amount of immune-conjugates that decreased the peak current. The incubation time and concentration of the antibody was optimized for better analytical performance of the immunosensor. The developed amperometric immunosensor is sensitive to IgG concentration as low as 2 ng/mL. Tailoring of redox-active dendrimers provides enhanced electroactivity to the system and enlarges the sensor surface for binding the antibodies. It may be assumed that both electron transfer and diffusion contribute to the signal transformation between the dendrimers and the antibody.

Keywords: ferrocenyl dendrimers, electrochemical immunosensors, immunoglobulin, amperometry

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Authors: Albert Mufundirwa, Satoru Yoshioka, K. Ogi, Takeharu Sugiyama, George F. Harrington, Bretislav Smid, Benjamin Cunning, Kazunari Sasaki, Akari Hayashi, Stephen M. Lyth

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Polymer electrolyte membrane fuel cells (PEMFCs) are electrochemical energy conversion devices used for portable, residential and vehicular applications due to their low emissions, high efficiency, and quick start-up characteristics. However, PEMFCs generally use expensive, Pt-based electrocatalysts as electrode catalysts. Due to the high cost and limited availability of platinum, research and development to either drastically reduce platinum loading, or replace platinum with alternative catalysts is of paramount importance. A combination of high surface area supports and nano-structured active sites is essential for effective operation of catalysts. We synthesize carbon foam supports by thermal decomposition of sodium ethoxide, using a template-free, gram scale, cheap, and scalable pyrolysis method. This carbon foam has a high surface area, highly porous, three-dimensional framework which is ideal for electrochemical applications. These carbon foams can have surface area larger than 2500 m²/g, and electron microscopy reveals that they have micron-scale cells, separated by few-layer graphene-like carbon walls. We applied this carbon foam as a platinum catalyst support, resulting in the improved electrochemical surface area and mass activity for the oxygen reduction reaction (ORR), compared to carbon black. Similarly, silver-decorated carbon foams showed higher activity and efficiency for electrochemical carbon dioxide conversion than silver-decorated carbon black. A promising alternative to Pt-catalysts for the ORR is iron-impregnated nitrogen-doped carbon catalysts (Fe-N-C). Doping carbon with nitrogen alters the chemical structure and modulates the electronic properties, allowing a degree of control over the catalytic properties. We have adapted our synthesis method to produce nitrogen-doped carbon foams with large surface area, using triethanolamine as a nitrogen feedstock, in a novel bottom-up protocol. These foams are then infiltrated with iron acetate (FeAc) and pyrolysed to form Fe-N-C foams. The resulting Fe-N-C foam catalysts have high initial activity (half-wave potential of 0.68 VRHE), comparable to that of commercially available Pt-free catalysts (e.g., NPC-2000, Pajarito Powder) in acid solution. In alkaline solution, the Fe-N-C carbon foam catalysts have a half-wave potential of 0.89 VRHE, which is higher than that of NPC-2000 by almost 10 mVRHE, and far out-performing platinum. However, the durability is still a problem at present. The lessons learned from X-ray absorption spectroscopy (XAS), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and electrochemical measurements will be used to carefully design Fe-N-C catalysts for higher performance PEMFCs.

Keywords: carbon-foam, polymer electrolyte membrane fuel cells, platinum, Pt-free, Fe-N-C, ORR

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Authors: Neumoin Anton Ivanovich, Opra Denis Pavlovich

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Materials based on titanium oxide compounds are widely used in such areas as solar energy, photocatalysis, food industry and hygiene products, biomedical technologies, etc. Demand for them has also formed in the battery industry (an example of this is the commercialization of Li4Ti5O12), where much attention has recently been paid to the development of next-generation systems and technologies, such as sodium-ion batteries. This dictates the need to search for new materials with improved characteristics, as well as ways to obtain them that meet the requirements of scalability. One of the ways to solve these problems can be the creation of nanomaterials that often have a complex of physicochemical properties that radically differ from the characteristics of their counterparts in the micro- or macroscopic state. At the same time, it is important to control the texture (specific surface area, porosity) of such materials. In view of the above, among other methods, the hydrothermal technique seems to be suitable, allowing a wide range of control over the conditions of synthesis. In the present study, a method was developed for the preparation of mesoporous nanostructured sodium trititanate (Na2Ti3O7) with a hierarchical architecture. The materials were synthesized by hydrothermal processing and exhibit a complex hierarchically organized two-layer architecture. At the first level of the hierarchy, materials are represented by particles having a roughness surface, and at the second level, by one-dimensional nanotubes. The products were found to have high specific surface area and porosity with a narrow pore size distribution (about 6 nm). As it is known, the specific surface area and porosity are important characteristics of functional materials, which largely determine the possibilities and directions of their practical application. Electrochemical impedance spectroscopy data show that the resulting sodium trititanate has a sufficiently high electrical conductivity. As expected, the synthesized complexly organized nanoarchitecture based on sodium trititanate with a porous structure can be practically in demand, for example, in the field of new generation electrochemical storage and energy conversion devices.

Keywords: sodium trititanate, hierarchical materials, mesoporosity, nanotubes, hydrothermal synthesis

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Authors: Nathalia Florencia Barros Azeredo, Josué Martins Gonçalves, Pamela De Oliveira Rossini, Koiti Araki, Lucio Angnes

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This work demonstrates the electroanalysis of uric acid (UA) at very low working potential (0 V vs Ag/AgCl) directly in body fluids such as saliva and sweat using electrodes modified with mixed -Ni0.75Zn0.25(OH)2 nanoparticles exhibiting stable electrocatalytic responses from alkaline down to weakly acidic media (pH 14 to 3 range). These materials were prepared for the first time and fully characterized by TEM, XRD, and spectroscopic techniques. The electrochemical properties of the modified electrodes were evaluated in a fast and simple procedure for uric acid analyses based on cyclic voltammetry and chronoamperometry, pushing down the detection and quantification limits (respectively of 2.3*10-8 and 7.6*10-8 mol L-1) with good repeatability (RSD = 3.2% for 30 successive analyses pH 14). Finally, the possibility of real application was demonstrated upon realization of unexpectedly robust and sensitive modified FTO (fluorine doped tin oxide) glass and screen-printed sensors for measurement of uric acid directly in real saliva and sweat samples, with no significant interference of usual concentrations of ascorbic acid, acetaminophen, lactate and glucose present in those body fluids (Fig. 1).

Keywords: nickel hydroxide, mixed catalyst, uric acid sensors, biofluids

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Authors: Mandlenkosi G. R. Mahlobo, Peter A. Olubambi, Philippe Refait

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The aim of this study was to use voltammetry as a method to understand the behaviour of steel in unsaturated soil in the presence of cathodic protection (CP). Three carbon steel coupons were buried in artificial soil wetted at 65-70% of saturation for 37 days. All three coupons were left at open circuit potential (OCP) for the first seven days in the unsaturated soil before CP, which was only applied on two of the three coupons at the protection potential -0.8 V vs Cu/CuSO₄ for the remaining 30 days of the experiment. Voltammetry was performed weekly on the coupon without CP, while electrochemical impedance spectroscopy (EIS) was performed daily to monitor and correct the applied CP potential from the ohmic drop. Voltammetry was finally performed on the last day on the coupons under CP. All the voltammograms were modeled with mathematical equations in order to compute the electrochemical parameters and subsequently deduced the corrosion rate of the steel coupons. For the coupon without CP, the corrosion rate was determined at 300 µm/y. For the coupons under CP, the residual corrosion rate under CP was estimated at 12 µm/y while the corrosion rate of the coupons, after interruption of CP, was estimated at 25 µm/y. This showed that CP was efficient due to two effects: a direct effect from the decreased potential and an induced effect associated with the increased interfacial pH that promoted the formation of a protective layer on the steel surface.

Keywords: carbon steel, cathodic protection, voltammetry, unsaturated soil, Raman spectroscopy

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Authors: A. Sezai Sarac

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Acrylonitrile (AN) copolymers with typical comonomers of vinyl acetate (VAc) or methyl acrylate (MA) exhibit better mechanical behaviors than its homopolymer. To increase processability of conjugated polymer, and to obtain a hybrid nano-structure multi-stepped emulsion polymerization was applied. Such products could be used in, i.e., drug-delivery systems, biosensors, gas-sensors, electronic compounds, etc. Incorporation of a number of flexible comonomers weakens the dipolar interactions among CN and thereby decreases melting point or increases decomposition temperatures of the PAN based copolymers. Hence, it is important to consider the effect of comonomer on the properties of PAN-based copolymers. Acrylonitrile vinylacetate (AN–VAc ) copolymers have the significant effect to their thermal behavior and are also of interest as precursors in the production of high strength carbon fibers. AN is copolymerized with one or two comonomers, particularly with vinyl acetate The copolymer of AN and VAc can be used either as a plastic (VAc > 15 wt %) or as microfibers (VAc < 15 wt %). AN provides the copolymer with good processability, electrochemical and thermal stability; VAc provides the mechanical stability. The free radical copolymerization of AN and VAc copolymer and core Shell structure of polyprrole composites,and nanofibers of poly(m-anthranilic acid)/polyacrylonitrile blends were recently studied. Free radical copolymerization of acrylonitrile (AN) – with different comonomers, i.e. acrylates, and styrene was realized using ammonium persulfate (APS) in the presence of a surfactant and in-situ polymerization of conjugated polymers was performed in this reaction medium to obtain core-shell nano particles. Nanofibers of such nanoparticles were obtained by electrospinning. Morphological properties of nanofibers are investigated by scanning electron microscopy (SEM) and atomic force spectroscopy (AFM). Nanofibers are characterized using Fourier Transform Infrared - Attenuated Total Reflectance spectrometer (FTIR-ATR), Nuclear Magnetic Resonance Spectroscopy (1H-NMR), differential scanning calorimeter (DSC), thermal gravimetric analysis (TGA), and Electrochemical Impedance Spectroscopy. The electrochemical Impedance results of the nanofibers were fitted to an equivalent curcuit by modelling (ECM).

Keywords: core shell nanoparticles, nanofibers, ascrylonitile copolymers, hybrid nanostructures

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Authors: Meareg Amare, Senait Aklog

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Lignin film was deposited at the surface of the glassy carbon electrode potential-statically. In contrast to the unmodified glassy carbon electrode, an oxidative peak with an improved current and overpotential for caffeine at the modified electrode showed catalytic activity of the modifier towards oxidation of caffeine. Linear dependence of peak current on caffeine concentration in the range 6 × 10⁻⁶ to 100 × 10⁻⁶ mol L⁻¹ with determination coefficient and method detection limit (LoD = 3 s/slope) of 0.99925 and 8.37 × 10⁻⁷ mol L⁻¹, respectively, supplemented by recovery results of 93.79–102.17%, validated the developed method. An attempt was made to determine the caffeine content of aqueous coffee extracts of Ethiopian coffees grown in four coffee cultivating localities (Wonbera, Wolega, Finoteselam, and Zegie) and hence to evaluate the correlation between users preference and caffeine content. In agreement with reported works, caffeine contents (w/w%) of 0.164 in Wonbera coffee; 0.134 in Wolega coffee; 0.097 in Finoteselam coffee; and 0.089 in Zegie coffee were detected, confirming the applicability of the developed method for determination of caffeine in a complex matrix environment. The result indicated that users’ highest preference for Wonbera and least preference for Zegie cultivated coffees are in agreement with the caffeine content.

Keywords: electrochemical, lignin, caffeine, electrode

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Authors: Jinliang Yuan, Jong-Sung Yu, Bengt Sundén

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A computational fluid dynamics (CFD) model is developed for rechargeable non-aqueous electrolyte lithium-air batteries with a partial opening for oxygen supply to the cathode. Multi-phase transport phenomena occurred in the battery are considered, including dissolved lithium ions and oxygen gas in the liquid electrolyte, solid-phase electron transfer in the porous functional materials and liquid-phase charge transport in the electrolyte. These transport processes are coupled with the electrochemical reactions at the active surfaces, and effects of discharge reaction-generated solid Li2O2 on the transport properties and the electrochemical reaction rate are evaluated and implemented in the model. The predicted results are discussed and analyzed in terms of the spatial and transient distribution of various parameters, such as local oxygen concentration, reaction rate, variable solid Li2O2 volume fraction and porosity, as well as the effective diffusion coefficients. It is found that the effect of the solid Li2O2 product deposited at the solid active surfaces is significant on the transport phenomena and the overall battery performance.

Keywords: Computational Fluid Dynamics (CFD), modeling, multi-phase, transport phenomena, lithium-air battery

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Authors: Malek Mahmoudi, Jonas Keruckas, Dmytro Volyniuk, Jurate Simokaitiene, Juozas V. Grazulevicius

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Host materials have been discovered as one of the most appealing methods for harvesting triplet states in organic materials for application in organic light-emitting diodes (OLEDs). The ideal host-guest system for emission in thermally delayed fluorescence OLEDs with 20% guest concentration for efficient energy transfer has been demonstrated in the present investigation. In this work, 3,3'-bis[9-(4-fluorophenyl) carbazole] (bFPC) has been used as the host, which induces balanced charge carrier transport for high-efficiency OLEDs.For providing a complete characterization of the synthesized compound, photophysical, photoelectrical, charge-transporting, and electrochemical properties of the compound have been examined. Excited-state lifetimes and singlet-triplet energy gaps were measured for characterization of photophysical properties, while thermogravimetric analysis, as well as differential scanning calorimetry measurements, were performed for probing of electrochemical and thermal properties of the compound. The electrochemical properties of this compound were investigated by cyclic voltammetry (CV) method, and ionization potential (IPCV) value of 5.68 eV was observed. UV–Vis absorption and photoluminescence spectrum of a solution of the compound in toluene (10-5 M) showed maxima at 302 and 405 nm, respectively. Photoelectron emission spectrometry was used for the characterization of charge-injection properties of the studied compound in solid. The ionization potential of this material was found to be 5.78 eV, and time-of-flight measurement was used for testing charge-transporting properties and hole mobility estimated using this technique in a vacuum-deposited layer reached 4×10-4 cm2 V-1s-1. Since the compound with high charge mobilities was tested as a host in an organic light-emitting diode. The device was fabricated by successive deposition onto a pre-cleaned indium tin oxide (ITO) coated glass substrate under a vacuum of 10-6 Torr and consisting of an indium-tin-oxide anode, hole injection and transporting layer(MoO3, NPB), emitting layer with bFPC as a host and 4CzIPN (2,4,5,6-tetra(9-carbazolyl)isophthalonitrile) which is a new highly efficient green thermally activated delayed fluorescence (TADF) material as an emitter, an electron transporting layer(TPBi) and lithium fluoride layer topped with aluminum layer as a cathode exhibited the highest maximum current efficiency and power efficiency of 33.9 cd/A and 23.5 lm/W, respectively and the electroluminescence spectrum showed only a peak at 512nm. Furthermore, the new bicarbazole-based compound was tested as a host in thermally activated delayed fluorescence organic light-emitting diodes are reaching luminance of 25300 cd m-2 and external quantum efficiency of 10.1%. Interestingly, the turn-on voltage was low enough (3.8 V), and such a device can be used for highly efficient light sources.

Keywords: thermally-activated delayed fluorescence, host material, ionization energy, charge mobility, electroluminescence

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Authors: Siddhant Srivastav, Shilpa Singh, Sumanta Kumar Meher

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Innovative renewable energy sources for energy storage/conversion is the demand of the current scenario in electrochemical machinery. In this context, choosing suitable organic precipitants for tuning the crystal characteristics and microstructures is a challenge. On the same note, herein we report broccoli flower-like porous Mn3O4/NiSe2−MnSe2 composite synthesized using a simple two step hydrothermal synthesis procedure assisted by sluggish precipitating agent and an effective cappant followed by intermediated anion exchange. The as-synthesized material was exposed to physical and chemical measurements depicting poly-crystallinity, stronger bonding and broccoli flower-like porous arrangement. The material was assessed electrochemically by cyclic voltammetry (CV), chronopotentiometry (CP) and electrochemical impedance spectroscopy (EIS) measurements. The Electrochemical studies reveal redox behavior, supercapacitive charge-discharge shape and extremely low charge transfer resistance. Further, the fabricated Mn3O4/NiSe2−MnSe2 composite based solid-state hybrid supercapacitor (Mn3O4/NiSe2−MnSe2 ||N-rGO) delivers excellent rate specific capacity, very low internal resistance, with energy density (~34 W h kg–1) of a typical rechargeable battery and power density (11995 W kg–1) of an ultra-supercapacitor. Consequently, it can be a favorable contender for supercapacitor applications for high performance energy storage utilizations. A definitive exhibition of the supercapacitor device is credited to electrolyte-ion buffering reservior alike behavior of broccoli flower like Mn3O4/NiSe2−MnSe2, enhanced by upgraded electronic and ionic conductivities of N- doped rGO (negative electrode) and PVA/KOH gel (electrolyte separator), respectively

Keywords: electrolyte-ion buffering reservoir, intermediated-anion exchange, solid-state hybrid supercapacitor, supercapacitive charge-dischargesupercapacitive charge-discharge

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Authors: Lawrence I. Onyeji, Girish M. Kale, M. Bijan Kermani

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Corrosion problem which exists in every stage of oil and gas production has been a great challenge to the operators in the industry. The conventional carbon steel with all its inherent advantages has been adjudged susceptible to the aggressive corrosion environment of oilfield. This has aroused increased interest in the use of micro alloyed steels for oil and gas production and transportation. The corrosion behavior of three commercially supplied micro alloyed steels designated as A, B, and C have been investigated with API 5L X65 as reference samples. Electrochemical corrosion tests were conducted in an unbuffered 3.5 wt% NaCl solution saturated with CO₂ at 30 ⁰C for 24 hours. Pre-corrosion analyses revealed that samples A, B and X65 consist of ferrite-pearlite microstructures but with different grain sizes, shapes and distribution whereas sample C has bainitic microstructure with dispersed acicular ferrites. The results of the electrochemical corrosion tests showed that within the experimental conditions, the corrosion rate of the samples can be ranked as CR_(A)< CR_(X65)< CR_(B)< CR_(C). These results are attributed to difference in microstructures of the samples as depicted by ASTM grain size number in accordance with ASTM E112-12 Standard and ferrite-pearlite volume fractions determined by ImageJ Fiji grain size analysis software.

Keywords: carbon dioxide corrosion, corrosion behaviour, micro-alloyed steel, microstructures

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Authors: Z. Khalifa, K. M. Hassan, M. Abdel Azzem

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Potential strategies for deriving useful forms of renewable high density energy from abundant energy stored in carbohydrates is direct conversion of glucose (GLU) to electrical power. A three novel versatile modified electrodes, synthesized by electrochemical polymerization of organic monomers on glassy carbon electrodes (GC), have been developed for biofuel cells results in stable and long-term power production. Electrocatalytic oxidation of glucose in alkaline solution on conducting polymers electrodes modified by incorporation of Ni nanoparticles (NiNPs) onto poly(1,5-aminonaphthalene) (1,5-PDAN), poly(1,8-diaminonaphthalene) (1,8-PDAN) and poly(1-amino-2-methyl-9,10-anthraquinone) (PAMAQ) was investigated. The electrocatalytic oxidation of glucose at NiNPs-modified 1,5-PDAN/GC, 1,8-PDAN/GC and PAMAQ/GC electrodes has been studied using voltammetry technique. The PDAN electrodes show a slight activity in the potential of interest. The prepared NiNPs/PAMAQ/GC catalyst showed a very interesting catalytic activity that was nicely comparable to the NiNPs/1,5-PDAN/GC, NiNPs/1,8-PDAN/GC modified electrodes. In advance, both shows a significant more catalytic activity compared to the reported data for electrodes for glucose electrocatalytic oxidation.

Keywords: biofuel cells, glucose oxidation, electrocatalysis, nanoparticles and modified electrodes

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Authors: Yifan Fan, Xudong Luo, Pingping Lin

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An essential task in the field of artificial intelligence is to allow computers to interact with people through natural language. Therefore, researches such as virtual assistants and dialogue systems have received widespread attention from industry and academia. The response generation plays a crucial role in dialogue systems, so to push forward the research on this topic, this paper surveys various methods for response generation. We sort out these methods into three categories. First one includes finite state machine methods, framework methods, and instance methods. The second contains full-text indexing methods, ontology methods, vast knowledge base method, and some other methods. The third covers retrieval methods and generative methods. We also discuss some hybrid methods based knowledge and deep learning. We compare their disadvantages and advantages and point out in which ways these studies can be improved further. Our discussion covers some studies published in leading conferences such as IJCAI and AAAI in recent years.

Keywords: deep learning, generative, knowledge, response generation, retrieval

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Authors: Anteneh Wodaje Bayeh, Daniel Manaye Kabtamu, Chen-Hao Wang

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As one of the most promising electrochemical energy storage systems, vanadium redox flow batteries (VRFBs) have received increasing attention owing to their attractive features for largescale storage applications. However, their high production cost and relatively low energy efficiency still limit their feasibility. For practical implementation, it is of great interest to improve their efficiency and reduce their cost. One of the key components of VRFBs that can greatly influence the efficiency and final cost is the electrode, which provide the reactions sites for redox couples (VO²⁺/VO₂ + and V²⁺/V³⁺). Carbon-based materials are considered to be the most feasible electrode materials in the VRFB because of their excellent potential in terms of operation range, good permeability, large surface area, and reasonable cost. However, owing to limited electrochemical activity and reversibility and poor wettability due to its hydrophobic properties, the performance of the cell employing carbon-based electrodes remained limited. To address the challenges, we synthesized heteroatom-doped bimetallic oxide grown on the surface of carbon through the one-step approach. When applied to VRFBs, the prepared electrode exhibits significant electrocatalytic effect toward the VO²⁺/VO₂ + and V³⁺/V²⁺ redox reaction compared with that of pristine carbon. It is found that the presence of heteroatom on metal oxide promotes the absorption of vanadium ions. The controlled morphology of bimetallic metal oxide also exposes more active sites for the redox reaction of vanadium ions. Hence, the prepared electrode displays the best electrochemical performance with energy and voltage efficiencies of 74.8% and 78.9%, respectively, which is much higher than those of 59.8% and 63.2% obtained from the pristine carbon at high current density. Moreover, the electrode exhibit durability and stability in an acidic electrolyte during long-term operation for 1000 cycles at the higher current density.

Keywords: VRFB, VO²⁺/VO₂ + and V³⁺/V²⁺ redox couples, graphite felt, heteroatom-doping

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Authors: Kathleen Moyer, Nora Ait Boucherbil, Murtaza Zohair, Janna Eaves-Rathert, Cary Pint

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This study demonstrates the significance of interface engineering in the field of structural energy by being the first case where the performance of the system with the structural battery is greater than the performance of the same system with a battery separate from the system. The benefits of improving the interface in the structural battery were tested by creating carbon fiber composite batteries (and independent graphite electrodes and lithium iron phosphate electrodes) with and without an improved interface. Mechanical data on the structural batteries were collected using tensile tests and electrochemical data was collected using scanning electron microscopy equipment. The full-cell lithium-ion structural batteries had capacity retention of over 80% exceeding 100 cycles with an average energy density of 52 W h kg−1 and a maximum energy density of 58 W h kg−1. Most scientific developments in the field of structural energy have been done with supercapacitors. Most scientific developments with structural batteries have been done where batteries are simply incorporated into the structural element. That method has limited advantages and can create mechanical disadvantages. This study aims to show that a large improvement in structure energy research can be made by improving the interface between the structural device and the battery.

Keywords: composite materials, electrochemical performance, mechanical properties, polymer interface, structural batteries

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Authors: G. Kaur, A. P. Kulkarni, S. Giddey

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Production of fuels and chemicals using renewable energy is a promising way for large-scale energy storage and export. Solid oxide electrolysers (SOEs) integrated with renewable source of energy can produce 'Syngas' H₂/CO from H₂O/CO₂ in the desired ratio for further conversion to liquid fuels. As only a waste CO₂ from industrial and power generation processes is utilized in these processes, this approach is CO₂ neutral compared to using fossil fuel feedstock. In addition, the waste heat from industrial processes or heat from solar thermal concentrators can be effectively utilised in SOEs to further reduce the electrical requirements by up to 30% which boosts overall energy efficiency of the process. In this paper, the electrochemical performance of various novel steam/CO₂ reduction electrodes (cathode) would be presented. The efficiency and lifetime degradation data for single cells and a stack would be presented along with the response of cells to variable electrical load input mimicking the intermittent nature of the renewable energy sources. With such optimisation, newly developed electrodes have been tested for 500+ hrs with Faraday efficiency (electricity to fuel conversion efficiency) up to 95%, and thermal efficiency in excess of 70% based upon energy content of the syngas produced.

Keywords: carbon dioxide, steam conversion, electrochemical system, energy storage, fuel production, renewable energy

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Authors: Simrjit Singh, Neeraj Khare

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In recent years, photo-electrochemical (PEC) water splitting with an aim to generate hydrogen (H₂) as a clean and renewable fuel has been the subject of intense research interests. Ferroelectric semiconductors have been demonstrated to exhibit enhanced PEC properties as these can be polarized with the application of an external electric field resulting in a built-in potential which helps in separating out the photogenerated charge carriers. In addition to this, by changing the polarization direction, the energy band alignment at the electrode/electrolyte interface can be modulated in a way that it can help in the easy transfer of the charge carriers from the electrode to the electrolyte. In this paper, we investigated the photoelectrochemical properties of ferroelectric PVDF/Cu/PVDF-NaNbO₃ PEC cell and demonstrated that PEC properties can be tuned with ferroelectric polarization and piezophototronic effect. Photocurrent density is enhanced from ~0.71 mA/cm² to 1.97 mA/cm² by changing the polarization direction. Furthermore, due to flexibility and piezoelectric properties of PVDF/Cu/PVDF-NaNbO₃ PEC cell, a further ~26% enhancement in the photocurrent is obtained using the piezophototronic effect. A model depicting the modulation of band alignment between PVDF and NaNbO₃ with the electric field is proposed to explain the observed tuning of the PEC properties. Electrochemical Impedance spectroscopy measurements support the validity of the proposed model.

Keywords: electrical tuning, H₂ generation, photoelectrochemical, NaNbO₃

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Authors: Christian C. Vaso, Rinlee Butch M. Cervera

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One of the most promising anode materials for solid oxide electrolysis cell (SOEC) application is the Sr-doped LaMnO₃ (LSM) which is known to have a high electronic conductivity but low ionic conductivity. To increase the ionic conductivity or diffusion of ions through the anode, Yttria-stabilized Zirconia (YSZ), which has good ionic conductivity, is proposed to be combined with LSM to create a composite electrode and to obtain a high mixed ionic and electronic conducting anode. In this study, composite of lanthanum strontium manganite and YSZ oxide, La_0.8Sr_0.2MnO₃/Zr_0.92Y_0.08O₂ (LSM/YSZ), with different wt.% compositions of LSM and YSZ were synthesized using solid-state reaction. The obtained prepared composite samples of 60, 50, and 40 wt.% LSM with remaining wt.% of 40, 50, and 60, respectively for YSZ were fully characterized for its microstructure by using powder X-ray diffraction (XRD), Thermogravimetric analysis (TGA), Fourier transform infrared (FTIR), and Scanning electron microscope/Energy dispersive spectroscopy (SEM/EDS) analyses. Surface morphology of the samples via SEM analysis revealed a well-sintered and densified pure LSM, while a more porous composite sample of LSM/YSZ was obtained. Electrochemical impedance measurements at intermediate temperature range (500-700 °C) of the synthesized samples were also performed which revealed that the 50 wt.% LSM with 50 wt.% YSZ (L50Y50) sample showed the highest total conductivity of 8.27x10^-1 S/cm at 600 ^oC with 0.22 eV activation energy.

Keywords: ceramics, microstructure, fuel cells, electrochemical impedance spectroscopy

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Authors: Wenjun Zhang, Thao Thi Le, Dongyup Shin, Jong Min Kim

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Electrochemical hydrogen peroxide (H₂O₂) synthesis holds significant promise for decentralized environmental remediation through the electro-Fenton process. However, challenges persist, such as the absence of robust electrocatalysts for the selective two-electron oxygen reduction reaction (2e⁻ ORR) and the high cost and sluggish kinetics of conventional electro-Fenton systems in treating highly concentrated wastewater. This study introduces an efficient water treatment system for removing substantial quantities of organic pollutants using an advanced electro-Fenton system coupled with a high-valent NiO catalyst. By employing a precipitation method involving crystal facet and cation vacancy engineering, a trivalent Ni (Ni³⁺)-rich NiO catalyst with a (111)-domain-exposed crystal facet, named {111}-NivO, was synthesized. This catalyst exhibited a remarkable 96% selectivity and a high mass activity of 59 A g⁻¹ for H₂O₂ production, outperforming all previously reported Ni-based catalysts. Furthermore, an advanced electro-Fenton system, integrated with a flow cell for electrochemical H₂O₂ production, was utilized to achieve 100% removal of 50 ppm bisphenol A (BPA) in 200 mL of wastewater under heavy-duty conditions, reaching a superior rapid degradation rate (4 min, k = 1.125 min⁻¹), approximately 102 times faster than the conventional electro-Fenton system. The hyper-efficiency is attributed to the continuous and appropriate supply of H₂O₂, the provision of O₂, and the timely recycling of the electrolyte under high current density operation. This catalyst also demonstrated a 93% removal of total organic carbon after 2 hours of operation and can be applied for efficient removal of highly concentrated phenol pollutants from aqueous systems, which opens new avenues for wastewater treatment.

Keywords: hydrogen peroxide production, nickel oxides, crystal facet and cation vacancy engineering, wastewater treatment, flow cell, electro-Fenton

Procedia PDF Downloads 23

Authors: Gabriel Wosiak, Dyovani Coelho, Evaldo B. Carneiro-Neto, Ernesto C. Pereira, Mauro C. Lopes

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In this work, the theoretical and experimental effects of induced charging currents on fast-scan cyclic voltammetry (FSCV) are investigated. Induced charging currents arise from the effect of ohmic drop in electrochemical systems, which depends on the presence of an uncompensated resistance. They cause the capacitive contribution to the total current to be different from the capacitive current measured in the absence of electroactive species. The paper shows that the induced charging current is relevant when the capacitive current magnitude is close to the total current, even for systems with low time constant. In these situations, the conventional background subtraction method may be inaccurate. A method is developed that separates the faradaic and capacitive currents by using a combination of voltametric experimental data and finite element simulation, by the obtention of a potential-dependent capacitance. The method was tested in a standard electrochemical cell with Platinum ultramicroelectrodes, in different experimental conditions as well in previously reported data in literature. The proposed method allows the real capacitive current to be separated even in situations where the conventional background subtraction method is clearly inappropriate.

Keywords: capacitive current, fast-scan cyclic voltammetry, finite-element method, electroanalysis

Procedia PDF Downloads 45

Authors: Feixiong Chen, Naoufel Haddour, Marie Frenea-Robin, Yves MéRieux, Yann Chevolot, Virginie Monnier

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Neonatal thrombopenia occurs when the mother generates antibodies against her baby’s platelet antigens. It is particularly critical for newborns because it can cause coagulation troubles leading to intracranial hemorrhage. In this case, diagnosis must be done quickly to make platelets transfusion immediately after birth. Before transfusion, platelet antigens must be tested carefully to avoid rejection. The majority of thrombopenia (95 %) are caused by antibodies directed against Human Platelet Antigen 1a (HPA-1a) or 5b (HPA-5b). The common method for antigen platelets detection is polymerase chain reaction allowing for identification of gene sequence. However, it is expensive, time-consuming and requires significant blood volume which is not suitable for newborns. We propose to develop a point-of-care device based on double functionalized magnetic colloids with 1) antibodies specific to antigen platelets and 2) highly sensitive electroactive molecules in order to be detected by an electrochemical microsensor. These magnetic colloids will be used first to isolate platelets from other blood components, then to capture specifically platelets bearing HPA-1a and HPA-5b antigens and finally to attract them close to sensor working electrode for improved electrochemical signal. The expected advantages are an assay time lower than 20 min starting from blood volume smaller than 100 µL. Our functionalization procedure based on amine dendrimers and NHS-ester modification of initial carboxyl colloids will be presented. Functionalization efficiency was evaluated by colorimetric titration of surface chemical groups, zeta potential measurements, infrared spectroscopy, fluorescence scanning and cyclic voltammetry. Our results showed that electroactive molecules and antibodies can be immobilized successfully onto magnetic colloids. Application of a magnetic field onto working electrode increased the detected electrochemical signal. Magnetic colloids were able to capture specific purified antigens extracted from platelets.

Keywords: Magnetic Nanoparticles , Electroactive Molecules, Antibody, Platelet

Procedia PDF Downloads 240

Authors: A. N. Fouda

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A novel well identified hexagonal graphene oxide (GO) nano-sheets were synthesized using modified Hummer method. Low temperature thermal reduction at 350°C in air ambient was performed. After thermal reduction, typical few layers of thermal reduced GO (TRGO) with dimension of few hundreds nanometers were observed using high resolution transmission electron microscopy (HRTEM). GO has a lot of structure models due to variation of the preparation process. Determining the atomic structure of GO is essential for a better understanding of its fundamental properties and for realization of the future technological applications. Structural characterization was identified by x-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FTIR) measurements. A comparison between exper- imental and theoretical IR spectrum were done to confirm the match between experimentally and theoretically proposed GO structure. Partial overlap of the experimental IR spectrum with the theoretical IR was confirmed. The electrochemical properties of TRGO nano-sheets as electrode materials for supercapacitors were investigated by cyclic voltammetry and electrochemical impedance spectroscopy (EIS) measurements. An enhancement in supercapacitance after reduction was confirmed and the area of the CV curve for the TRGO electrode is larger than those for the GO electrode indicating higher specific capacitance which is promising in super-capacitor applications

Keywords: hexagonal graphene oxide, thermal reduction, cyclic voltammetry

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Authors: Azeez O. Idris, Benjamin O. Orimolade, Potlako J. Mafa, Alex T. Kuvarega, Usisipho Feleni, Bhekie B. Mamba

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We report a simple and cheaper method for the electrochemical detection of Se(IV) using carbon nanodots (CNDTs) prepared from oat. The carbon nanodots were synthesised by green and facile approach and characterised using scanning electron microscopy, high-resolution transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, and Raman spectroscopy. The CNDT was used to fabricate an electrochemical sensor for the quantification of Se(IV) in water. The modification of glassy carbon electrode (GCE) with carbon nanodots led to an increase in the electroactive surface area of the electrode, which enhances the redox current peak of [Fe(CN)₆]₃₋/₄‒ in comparison to the bare GCE. Using the square wave voltammetry, the detection limit and quantification limit of 0.05 and 0.167 ppb were obtained under the optimised parameters using deposition potential of -200 mV, 0.1 M HNO₃ electrolyte, electrodeposition time of 60 s, and pH 1. The results further revealed that the GCE-CNDT was not susceptible to many interfering cations except Cu(II) and Pb(II), and Fe(II). The sensor fabrication involves a one-step electrode modification and was used to detect Se(IV) in a real water sample, and the result obtained is in agreement with the inductively coupled plasma technique. Overall, the electrode offers a cheap, fast, and sensitive way of detecting selenium in environmental matrices.

Keywords: carbon nanodots, square wave voltammetry, nanomaterials, selenium, sensor

Procedia PDF Downloads 63

Authors: H. Beisch, J. Marx, S. Garlof, R. Shvets, I. I. Grygorchak, A. Kityk, B. Fiedler

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Carbon materials, especially three-dimensional carbon foams, show very high potential in the application as electrode material for energy storage systems such as batteries and supercapacitors with unique fast charging and discharging times. Regarding their high specific surface areas (SSA) high specific capacities can be reached. Globugraphite is a newly developed carbon foam with an interconnected globular carbon morphology. Especially, this foam has a statistically distributed hierarchical pore structure resulting from the manufacturing process based on sintered ceramic templates which are synthetized during a final chemical vapor deposition (CVD) process. For morphology characterization scanning electron (SEM) and transmission electron microscopy (TEM) is used. In addition, the SSA is carried out by nitrogen adsorption combined with the Brunauer–Emmett–Teller (BET) theory. Electrochemical measurements in organic and inorganic electrolyte provide high energy densities and power densities resulting from ion absorption by forming an electrochemical double layer. All values are summarized in a Ragone Diagram. Finally, power densities up to 833 W/kg and energy densities up to 48 Wh/kg could be achieved. The corresponding SSA is between 376 m²/g and 859 m²/g. For organic electrolyte a specific capacity of 71 F/g at a density of 20 mg/cm³ was achieved.

Keywords: BET, CVD process, electron microscopy, Ragone diagram

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Authors: Hamide Aydin, Banu Karaman, Ayhan Bozkurt, Umran Kurtan

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Recently, Proton Conducting Gel Polymer Electrolytes (GPEs) have drawn much attention in supercapacitor applications due to their physical and electrochemical characteristics and stability conditions for low temperatures. In this research, PVA-H2SO4-H3BO3 GPE has been used for electric-double layer capacitor (EDLCs) application, in which electrospun free-standing carbon nanofibers are used as electrodes. Introduced PVA-H2SO4-H3BO3 GPE behaves as both separator and the electrolyte in the supercapacitor. Symmetric Swagelok cells including GPEs were assembled via using two electrode arrangements and the electrochemical properties were searched. Electrochemical performance studies demonstrated that PVA-H2SO4-H3BO3 GPE had a maximum specific capacitance (Cs) of 134 F g-1 and showed great capacitance retention (%100) after 1000 charge/discharge cycles. Furthermore, PVA-H2SO4-H3BO3 GPE yielded an energy density of 67 Wh kg-1 with a corresponding power density of 1000 W kg-1 at a current density of 1 A g-1. PVA-H2SO4 based polymer electrolyte was produced according to following procedure; Firstly, 1 g of commercial PVA was dissolved in distilled water at 90°C and stirred until getting transparent solution. This was followed by addition of the diluted H2SO4 (1 g of H2SO4 in a distilled water) to the solution to obtain PVA-H2SO4. PVA-H2SO4-H3BO3 based polymer electrolyte was produced by dissolving H3BO3 in hot distilled water and then inserted into the PVA-H2SO4 solution. The mole fraction was arranged to ¼ of the PVA repeating unit. After the stirring 2 h at RT, gel polymer electrolytes were obtained. The final electrolytes for supercapacitor testing included 20% of water in weight. Several blending combinations of PVA/H2SO4 and H3BO3 were studied to observe the optimized combination in terms of conductivity as well as electrolyte stability. As the amount of boric acid increased in the matrix, excess sulfuric acid was excluded due to cross linking, especially at lower solvent content. This resulted in the reduction of proton conductivity. Therefore, the mole fraction of H3BO3 was chosen as ¼ of PVA repeating unit. Within this optimized limits, the polymer electrolytes showed better conductivities as well as stability.

Keywords: electrical double layer capacitor, energy density, gel polymer electrolyte, ultracapacitor

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Authors: M. Zare, S. Biau, M. Corq, Y. Roquelaure

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A wide variety of observational methods have been developed to evaluate the ergonomic workloads in manufacturing. However, the precision and accuracy of these methods remain a subject of debate. The aims of this study were to develop biomechanical methods to evaluate ergonomic workloads and to compare them with observational methods. Two observational methods, i.e. SCANIA Ergonomic Standard (SES) and Rapid Upper Limb Assessment (RULA), were used to assess ergonomic workloads at two simulated workstations. They included four tasks such as tightening & loosening, attachment of tubes and strapping as well as other actions. Sensors were also used to measure biomechanical data (Inclinometers, Accelerometers, and Goniometers). Our findings showed that in assessment of some risk factors both RULA & SES were in agreement with the results of biomechanical methods. However, there was disagreement on neck and wrist postures. In conclusion, the biomechanical approach was more precise than observational methods, but some risk factors evaluated with observational methods were not measurable with the biomechanical techniques developed.

Keywords: ergonomic, observational method, biomechanical methods, workload

Procedia PDF Downloads 356