Search results for: electrochemical impedance spectra

Authors: Aicha Chaouay, Lahsen Bazzi, Mustapha Hilali

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Seawater has chemical and biological characteristics making it particularly aggressive in relation to the corrosion of many materials including copper and steels low or moderate allies. Note that these materials are widely used in the manufacture of port infrastructure in the marine environment. These structures are exposed to two types of corrosion including: general corrosion and localized corrosion caused by the presence of sulfite-reducing micro-organisms. This work contributes to the study of the problematic related to bacterial contamination of the marine environment of large Agadir and evaluating the impact of this pollution on the corrosion resistance of copper. For the realization of this work, we conducted monthly periodic draws between (October 2012 February 2013) of seawater from the Anza area of the Bay of Agadir. Thus, after each sampling, a study of the electro chemical corrosion behavior of copper was carried out. Electro chemical corrosion parameters such as the corrosion potential, the corrosion current density, the charge transfer resistance and the double layer capacity were evaluated. The electro chemical techniques used in this work are: the route potentiodynamic polarization curves and electro chemical impedance.

Keywords: Bay of Agadir, microbial contamination, seawater (Morocco), corrosion, copper

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Authors: P. Mirahmadpour, M. H. Banitaba, D. Nematollahi

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The chemistry of coordination polymers in recent years has grown exponentially not only because of their interesting architectures but also due to their various technical applications in many fields including ion exchange, chemical catalysis, small molecule separations, and drug release. The use of bridging ligands for the controlled self-assembly of one, two or three dimensional metallo-supramolecular species is the subject of serious study in last decade. Numerous different synthetic methods have been offered for the preparation of coordination polymers such as (a) diffusion from the gas phase, (b) slow diffusion of the reactants into a polymeric matrix, (c) evaporation of the solvent at ambient or reduced temperatures, (d) temperature controlled cooling, (e) precipitation or recrystallisation from a mixture of solvents and (f) hydrothermal synthesis. The electrosynthetic process suggested several advantages over conventional approaches. A general advantage of electrochemical synthesis is that it allows synthesis under milder conditions than typical solvothermal or microwave synthesis. In this work we have introduced a simple electrochemical method for growing metal coordination polymers based on copper with a flexible 2,2’-thiodiacetic acid (TDA) and rigid 1,2,4,5-benzenetetracarboxylate (BTC) ligands. The structure of coordination polymers were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), elemental analysis, thermal gravimetric (TG) and differential thermal analyses (DTA). The single-crystal X-ray diffraction analysis revealed that different conformations of the ligands and different coordination modes of the carboxylate group as well as different coordination geometries of the copper atoms. Electrochemical synthesis of coordination polymers has different advantages such as faster synthesis at lower temperature in compare with conventional chemical methods and crystallization of desired materials in a single synthetic step.

Keywords: 1, 2, 4, 5-benzenetetracarboxylate, coordination polymer, copper, 2, 2’-thiodiacetic acid

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Authors: M. Said Ahmed, M. Lebrini, J. Pellé, S. Rioual, B. Lescop, C. Roos

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The corrosion behavior of copper exposed in a marine atmosphere polluted and unpolluted by gases, mainly hydrogen sulphide (H2S), from the decomposition of Sargassum algae was studied using the mass loss method and electrochemical measurements. MEB/EDX and XRD were also used for the observation of morphology and surface analysis. To study the impact of this on copper corrosion, four sites more or less impacted by Sargassum algae strandings were selected. The samples were exposed for up to six months. The mass loss results showed that the average corrosion rate of copper was 528 µm/year for the site most affected by Sargassum algae and 9.4 µm/year for the least impacted site after three months of exposure, implying that the presence of Sargassum algae caused an important copper degradation. The morphological structures and properties of the corrosion products obtained at the impacted and non-impacted sites differed significantly. In the absence of Sargassum algae, we obtained mainly Cu2O and Cu2Cl(OH)3. Whereas in the atmosphere with Sargassum algae, CuS product is the main corrosion product obtained. Electrochemical analyses showed that the protection offered by the corrosion product layer was more important and improved with time for the non-impacted sites, whereas on the impacted sites, this protection deteriorated.

Keywords: atmospheric-corrosion, sargassum algae, copper, electrochemical techniques, SEM/EDX and XRD

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Authors: Kanta Maan Sangwan, Neetu Ahlawat, Rajender Singh Kundu

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BaZrTiO3 ceramics having high dielectric constant and low dielectric loss are interesting material for being used as commercial capacitor applications. BZT (BaZrTiO3) has attracted attentions for their many applications for the microwave technology as the doping of Zr4+ on Ti4+ has advantage to the stability of the system. In the present work, co-doping of Zr and V with BaTiO3 ceramics was synthesized by the conventional solid state reaction technique and sintered at 1200 K for 6 hours, and their structural and ferroelectric properties were studied. The XRD (x-ray diffraction) pattern of BZT (BaZrTiO3) ceramics shows that the crystalline sample is single phase tetragonal structure with P4mm space group. The result revealed that Zr ion enters the unit cell maintaining the perovskite structure of BZT ceramics and the impedance spectroscopy of the sample performed in selected frequency and temperature range.

Keywords: ferroelectric, impedance spectroscopy, space group, tetragonal

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Authors: Mao Li, Yuguang Ma, Katsuhiko Ariga

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The performance of functional materials is governed by their ability to interact with surrounding environments in a well-defined and controlled manner. Layer-by-Layer (LbL) assembly is one of the most widely used technologies for coating both planar and particulate substrates in a diverse range of fields, including optics, energy, catalysis, separations, and biomedicine. Herein, we introduce electrochemical-coupling layer-by-layer assembly as a novel fabrication methodology for preparing layered thin films. This assembly method not only determines the process properties (such as the time, scalability, and manual intervention) but also directly control the physicochemical properties of the films (such as the thickness, homogeneity, and inter- and intra-layer film organization), with both sets of properties linked to application-specific performance.

Keywords: layer by layer assembly, electropolymerization, carbazole, optical thin film, electronics

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Authors: J. Tomilla Ajayi, Werner E. Van Zyl

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This work presents an overview of the reaction of 2, 4-diferrocenyl-1, 3-dithiadiphosphetane-2, 4-disulfide (Ferrocenyl Lawesson’s reagent) with water to produce the non-symmetric, ferocenyl dithiophosphonic acid respectively in high yields. These acids were readily deprotonated by anhydrous Ammonia to yield the corresponding ammonium salt NH4S2PFcOH. These were complex to Ni (II) in molar ratio 1:1 and 1:2. The resulting complex from the reaction formed same compound with different isomers (Cis and Trans) and also compound with multimetallic coordination. Quality X-ray crystals were formed from THF/Ether. The compounds were characterized by 1H, 31P NMR, and FTIR. Bulk purity were confirmed by either ESI-MS or elemental analysis and The XRD images were obtained using single crystal X-ray crystallographic studies. The electrochemical investigation of the Compounds were carried out using cyclic voltammetry.

Keywords: ferrocenyl, dithiophosphonate, isomer, coordination

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Authors: Vinita Choudhary

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The solidly mounted resonator (SMR) is a bulk acoustic wave-based device consisting of a piezoelectric layer sandwiched between two electrodes upon Bragg reflectors, which then are attached to a substrate. To transform the effective acoustic impedance of the substrate to a near zero value, the Bragg reflectors are composed of alternating high and low acoustic impedance layers of quarter-wavelength thickness. In this work presents the design and investigation of acoustic Bragg reflectors (ABRs) for solidly mounted bulk acoustic wave resonators through analysis and simulation. This performance of the resonator is analyzed using 1D Mason modeling. The performance parameters are the effect of Bragg pairs number on transmissivity, reflectivity, insertion loss, the electromechanical and quality factor of the 5GHz operating resonator.

Keywords: bragg reflectors, SMR, insertion loss, quality factor

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Authors: Orsolya Kegyes-Brassai, Zsolt Szilvágyi, Ákos Wolf, Richard P. Ray

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Local ground conditions have a substantial influence on the seismic response of structures. Their inclusion in seismic hazard assessment and structural design can be realized at different levels of sophistication. However, response results based on more advanced calculation methods e.g. nonlinear or equivalent linear site analysis tend to show significant discrepancies when compared to simpler approaches. This project's main objective was to compare results from several 1-D response programs to Eurocode 8 design spectra. Data from in-situ site investigations were used for assessing local ground conditions at several locations in Hungary. After discussion of the in-situ measurements and calculation methods used, a comprehensive evaluation of all major contributing factors for site response is given. While the Eurocode spectra should account for local ground conditions based on soil classification, there is a wide variation in peak ground acceleration determined from 1-D analyses versus Eurocode. Results show that current Eurocode 8 design spectra may not be conservative enough to account for local ground conditions typical for Hungary.

Keywords: 1-D site response analysis, multichannel analysis of surface waves (MASW), seismic CPT, seismic hazard assessment

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Authors: Amin Asgarian, Ghyslaine McClure

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Proper seismic evaluation of Non-Structural Components (NSCs) mandates an accurate estimation of floor seismic demands (i.e. acceleration and displacement demands). Most of the current international codes incorporate empirical equations to calculate equivalent static seismic force for which NSCs and their anchorage system must be designed. These equations, in general, are functions of component mass and peak seismic acceleration to which NSCs are subjected to during the earthquake. However, recent studies have shown that these recommendations are suffered from several shortcomings such as neglecting the higher mode effect, tuning effect, NSCs damping effect, etc. which cause underestimation of the component seismic acceleration demand. This work is aimed to circumvent the aforementioned shortcomings of code provisions as well as improving them by proposing a simplified, practical, and yet accurate approach to generate acceleration Floor Design Spectra (FDS) directly from corresponding Uniform Hazard Spectra (UHS) (i.e. design spectra for structural components). A database of 27 Reinforced Concrete (RC) buildings in which Ambient Vibration Measurements (AVM) have been conducted. The database comprises 12 low-rise, 10 medium-rise, and 5 high-rise buildings all located in Montréal, Canada and designated as post-disaster buildings or emergency shelters. The buildings are subjected to a set of 20 compatible seismic records and Floor Response Spectra (FRS) in terms of pseudo acceleration are derived using the proposed approach for every floor of the building in both horizontal directions considering 4 different damping ratios of NSCs (i.e. 2, 5, 10, and 20% viscous damping). Several effective parameters on NSCs response are evaluated statistically. These parameters comprise NSCs damping ratios, tuning of NSCs natural period with one of the natural periods of supporting structure, higher modes of supporting structures, and location of NSCs. The entire spectral region is divided into three distinct segments namely short-period, fundamental period, and long period region. The derived roof floor response spectra for NSCs with 5% damping are compared with the 5% damping UHS and procedure are proposed to generate roof FDS for NSCs with 5% damping directly from 5% damped UHS in each spectral region. The generated FDS is a powerful, practical, and accurate tool for seismic design and assessment of acceleration-sensitive NSCs particularly in existing post-critical buildings which have to remain functional even after the earthquake and cannot tolerate any damage to NSCs.

Keywords: earthquake engineering, operational and functional components (OFCs), operational modal analysis (OMA), seismic assessment and design

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Authors: Dessie Tibebe, Muluken Asmare, Marye Mulugeta, Yezbie Kassa, Zerubabel Moges, Dereje Yenealem, Tarekegn Fentie, Agmas Amare

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The performance of electrocoagulation (EC) using Aluminium electrodes for the treatment of effluent-containing chromium metal using a fixed bed electrochemical batch reactor was studied. In the present work, the efficiency evaluation of EC in removing physicochemical and heavy metals from real industrial tannery wastewater in the Amhara region, collected from Bahirdar, Debre Brihan, and Haik, was investigated. The treated and untreated samples were determined by AAS and ICP OES spectrophotometers. The results indicated that selected heavy metals were removed in all experiments with high removal percentages. The optimal results were obtained regarding both cost and electrocoagulation efficiency with initial pH = 3, initial concentration = 40 mg/L, electrolysis time = 30 min, current density = 40 mA/cm2, and temperature = 25oC favored metal removal. The maximum removal percentages of selected metals obtained were 84.42% for Haik, 92.64% for Bahir Dar and 94.90% for Debre Brihan. The sacrificial electrode and sludge were characterized by FT-IR, SEM and XRD. After treatment, some metals like chromium will be used again as a tanning agent in leather processing to promote a circular economy.

Keywords: electrochemical, treatment, aluminum, tannery effluent

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Authors: Chia-Ting Chang, Chia-Yu Lin

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We report on the decisive role of iron phosphate (FePO₄), formed in-situ during the electrochemical characterization, played in the electrocatalytic activity, especially its oxygen tolerance of iron oxides towards H₂O₂ reduction. Iron oxides studied including, Nanorod arrays (NRs) of β-FeOOH, γ-Fe₂O₃, α-Fe₂O₃, α-Fe₂O₃ nanosheets (α-Fe₂O₃NS), α-Fe₂O₃ nanoparticles (α-Fe₂O₃NP), were synthesized using chemical bath deposition. The nanostructure was controlled simply by adjusting the composition of precursor solution and reaction duration for CBD process, whereas the crystal phase was controlled by adjusting the annealing temperature. It was found that iron phosphate (FePO₄) was deposited in-situ onto the surface of this nanostructured α-Fe₂O₃ during the electrochemical pretreatment in the phosphate electrolyte, and both FePO₄ and α-Fe₂O₃ showed the activity in catalysing the electrochemical reduction of H₂O₂. In addition, the interaction/compatibility between deposited FePO₄ and iron oxides has a decisive effect on the overall electrocatalytic activity of the resultant electrodes; FePO₄ only showed synergetic effect on the overall electrocatalytic activity of α-Fe₂O₃NR and α-Fe2O₃NS. Both α-Fe₂O₃NR and α-Fe₂O₃NS showed two reduction peaks in phosphate electrolyte containing H₂O₂, one being pH-dependent and related to the electrocatalytic properties of FePO₄, and the other one being pH-independent and only related to the intrinsic electrocatalytic properties of α-Fe₂O₃NR and α-Fe₂O₃NS. However, all iron oxides showed only one pH-independent reductive peak in non-phosphate electrolyte containing H₂O₂. The synergesitic catalysis exerted by FePO₄ with α-Fe₂O₃NR or α-Fe₂O₃NS providing additional oxygen-insensitive active site for H₂O₂ reduction, which allows their applications to electrochemical detection of H₂O₂ without the interference of O₂ involving in oxidase-catalyzed chemical processes.

Keywords: H₂O₂ reduction, Iron oxide, iron phosphate, O₂ tolerance

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Authors: R. Shrestha, D. P. Subedi, R. B. Tyata, C. S. Wong,

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In this paper, a technique for the determination of electron temperatures and electron densities in atmospheric pressure Argon/air discharge by the analysis of optical emission spectra (OES) is reported. The discharge was produced using a high voltage (0-20) kV power supply operating at a frequency of 27 kHz in parallel electrode system, with glass as dielectric. The dielectric layers covering the electrodes act as current limiters and prevent the transition to an arc discharge. Optical emission spectra in the range of (300nm-850nm) were recorded for the discharge with different inter electrode gap keeping electric field constant. Electron temperature (Te) and electron density (ne) are estimated from electrical and optical methods. Electron density was calculated using power balance method. The optical methods are related with line intensity ratio from the relative intensities of Ar-I and Ar-II lines in Argon plasma. The electron density calculated by using line intensity ratio method was compared with the electron density calculated by stark broadening method. The effect of dielectric thickness on plasma parameters (Te and ne) have also been studied and found that Te and ne increases as thickness of dielectric decrease for same inter electrode distance and applied voltage.

Keywords: electron density, electron temperature, optical emission spectra,

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Authors: Mahfouz Saeed

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Cu₂(ZnSn)(S)₄ (CTZS) offers potential advantages over CuInGaSe₂ (CIGS) as solar thin film because to its higher band gap. Preparing such photovoltaic materials by electrochemical techniques is particularly attractive due to the lower processing cost and the high throughput of such techniques. Several recent publications report CTZS electroplating; however, the electrochemical process still facing serious challenges such as a sulfur atomic ration which is about 50% of the total alloy. We introduce in this work an improved electrolyte composition which enables the direct electrodeposition of CTZS from a single bath. The electrolyte is significantly more dilute in comparison to common baths described in the literature. The bath composition we introduce is: 0.0032 M CuSO₄, 0.0021 M ZnSO₄, 0.0303 M SnCl₂, 0.0038 M Na₂S₂O₃, and 0.3 mM Na₂S₂O3. PHydrion is applied to buffer the electrolyte to pH=2, and 0.7 M LiCl is applied as supporting electrolyte. Electrochemical process was carried at a rotating disk electrode which provides quantitative characterization of the flow (room temperature). Comprehensive electrochemical behavior study at different electrode rotation rates are provided. The effects of agitation on atomic composition of the deposit and its adhesion to the molybdenum back contact are discussed. The post treatment annealing was conducted under sulfur atmosphere with no need for metals addition from the gas phase during annealing. The potential which produced the desired atomic ratio of CTZS at -0.82 V/NHE. Smooth deposit, with uniform composition across the sample surface and depth was obtained at 500 rpm rotation speed. Final sulfur atomic ratio was adjusted to 50.2% in order to have the desired atomic ration. The final composition was investigated using Energy-dispersive X-ray spectroscopy technique (EDS). XRD technique used to analyze CTZS crystallography and thickness. Complete and functional CTZS PV devices were fabricated by depositing all the required layers in the correct order and the desired optical properties. Acknowledgments: Case Western Reserve University for the technical help and for using their instruments.

Keywords: photovoltaic, CTZS, thin film, electrochemical

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Authors: Alvaro Ramírez, Martín Muñoz-Morales, Ester López- Fernández, Javier Llanos, C. Ania

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Carbon blacks are value-added materials typically produced through the incomplete combustion or thermal decomposition of hydrocarbons. Traditionally, they have been used as catalysts in many different applications, but in the last decade, their potential in green chemistry has gained significant attention. Among them, the electrochemical production of H₂O₂ has attracted interest because of their properties as high oxidant capacity or their industrial interest as a bleaching agent. Carbon blacks are commonly used in this application in a catalytic ink that is drop-casted on supporting electrodes and acts as catalysts for the electrochemical production of H₂O₂ through oxygen reduction reaction (ORR). However, the different structural and electrochemical behaviors of each type of carbon black influence their applications. In this line, the term ‘carbon black’, has to be considered as a generic name that does not guarantee any physicochemical properties if any further description is mentioned. In fact, different specific surface area (SSA), surface functional groups, porous structure, and electro catalysts effect seem very important for electrochemical applications, and considerable differences were found during the analysis of four types of carbon blacks. Thus, the aim of this work is to evaluate the influence of SSA, porous structure, oxygen functional groups, and structural defects to differentiate among these carbon blacks (e.g. Vulcan XC72, Superior Graphite Co, Printex XE2, and Prolabo) for H₂O₂ production via ORR, using carbon paper as electrode support with improved selectivity and efficiency. Results indicate that the number and size of pores, along with surface functional groups, are key parameters that significantly affect the overall process efficiency.

Keywords: carbon blacks, oxygen reduction reaction, hydrogen peroxide, porosity, surface functional groups

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Authors: Xinyong Li

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A new coupling system was constructed by combining photo-electrochemical cell with eletro-fenton cell (PEC-EF). The electrode material in this system was derived from MnyFe₁₋yCo Prussian-Blue-Analog (PBA). Mn₀.₄Fe₀.₆Co₀.₆₇-N@C spin-coated on carbon paper behaved as the gas diffusion cathode and Mn₀.₄Fe₀.₆Co₀.₆₇O₂.₂ spin-coated on fluorine-tin oxide glass (FTO) as anode. The two separated cells could degrade Sulfamethoxazole (SMX) simultaneously and some coupling mechanisms by PEC and EF enhancing the degradation efficiency were investigated. The continuous on-site generation of H₂O₂ at cathode through an oxygen reduction reaction (ORR) was realized over rotating ring-disk electrode (RRDE). The electron transfer number (n) of the ORR with Mn₀.₄Fe₀.₆Co₀.₆₇-N@C was 2.5 in the selected potential and pH range. The photo-electrochemical properties of Mn₀.₄Fe₀.₆Co₀.₆₇O₂.₂ were systematically studied, which displayed good response towards visible light. The photo-induced electrons at anode can transfer to cathode for further use. Efficient photo-electro-catalytic performance was observed in degrading SMX. Almost 100% SMX removal was achieved in 120 min. This work not only provided a highly effective technique for antibiotic treatment but also revealed the synergic effect between PEC and EF.

Keywords: Electro-Fenton, photo-electrochemical, synergic effect, sulfamethoxazole

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Authors: O. Tovide, N. Jahed, N. Mohammed, C. E. Sunday, H. R. Makelane, R. F. Ajayi, K. M. Molapo, A. Tsegaye, M. Masikini, S. Mailu, A. Baleg, T. Waryo, P. G. Baker, E. I. Iwuoha

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A graphenated–polyaniline (GR-PANI) nanocomposite sensor was constructed and used for the determination of anthracene. The direct electro-oxidation behavior of anthracene on the GR-PANI modified glassy carbon electrode (GCE) was used as the sensing principle. The results indicate thatthe response profile of the oxidation of anthracene on GR-PANI-modified GCE provides for the construction of sensor systems based onamperometric and potentiometric signal transductions. A dynamic linear range of 0.12- 100 µM anthracene and a detection limit of 0.044 µM anthracene were established for the sensor system.

Keywords: electrochemical sensors, environmental pollutants, graphenated-polymers, polyaromatic hydrocarbon

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Authors: L. N. Shubha, P. Madhusudana Rao

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The Polyaniline / Copper Oxide(PANI / CuO) nanocomposite was prepared by solution mixing of prepared Polyaniline and copper Oxide in Dimethyl sulfoxide (DMSO). The synthesis involved the formation of dark green colored Polyaniline-Copper Oxide nanocomposite. The synthesized polymer nano composites were characterized by XRD, FTIR, SEM and UV-Visible Spectroscopy. The characteristic peaks in XRD, FTIR and UV-Visible spectra confirmed the presence of CuO in the polymer structure. SEM analysis revealed formation of PANI/CuO nano composite The D.C. conductivity measurements were performed using two probe method for various temperatures.

Keywords: polyaniline/copper oxide (PANI/CuO) nanocomposite, XRD, SEM, FTIRand DC- conductivity, UV-visible spectra

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Authors: Behnoush Dousti, Ye Choi, Gil S. Lee

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Microsupercapacitors (MScs) are known as the future of miniaturized energy sources that can be coupled to a battery to deliver stable and constant energy to microelectronics. Among all their counterparts, electrochemical microsupercapacitor have drawn the most research attention due to their higher power density and long cycle life. Designing the microstructure and choosing the electroactive materials are two significant factors that greatly affect the performance of the device. Here, we report successful fabrication and characterization of a microsupercapacitor with interdigitated structure based on Carbon nanotube sheets (CNT sheet). Novel structure of highly aligned CNT sheet as the electrode materials which also offers excellent conductivity and large surface area along with doping with nitrogen, enabled us to develop a device with serval order of magnitude higher electrochemical performance than the pristine CNT in aqueous electrolyte including high specific capacitance and rate capabilities and excellent cycle life over 10000 cycles. Geometric parameters such as finger width and gap size were also studied and it was shown the device performance is much depended on them. Results of this study confirms the potential of CNT sheet for future energy storage devices.

Keywords: carbon nanotube, energy storage systems, microsupercapacitor, nitrogen doping

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Authors: Cherry Oo, Hnin Min Oo

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Software bug localization is one of the most costly tasks in program repair technique. Therefore, there is a high claim for automated bug localization techniques that can monitor programmers to the locations of bugs, with slight human arbitration. Spectrum-based bug localization aims to help software developers to discover bugs rapidly by investigating abstractions of the program traces to make a ranking list of most possible buggy modules. Using the Apache Commons Math library project, we study the diagnostic accuracy using our spectrum-based bug localization metric. Our outcomes show that the greater performance of a specific similarity coefficient, used to inspect the program spectra, is mostly effective on localizing of single line bugs.

Keywords: software testing, bug localization, program spectra, bug

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Authors: Amirhossein Hasani, Shamin Houshmand Sharifi

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In this work, we investigate humidity sensing behavior of the graphene oxide with porous silicon substrate. By evaporation method, aluminum interdigital electrodes have been deposited onto porous silicon substrate. Then, by drop-casting method graphene oxide solution was deposited onto electrodes. The porous silicon was formed by electrochemical etching. The experimental results showed that using porous silicon substrate, we obtained two times larger sensitivity and response time compared with the results obtained with silicon substrate without porosity.

Keywords: graphene oxide, porous silicon, humidity sensor, electrochemical

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Authors: H. Elmsellem, A. Aouniti, S. Radi, A. Chetouani, B. Hammouti

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The synthesis of new organic molecules offers various molecular structures containing heteroatoms and substituents for corrosion protection in acid pickling of metals. The most synthesized compounds are the nitrogen heterocyclic compounds, which are known to be excellent complex or chelate forming substances with metals. The choice of the inhibitor is based on two considerations: first it could be synthesized conveniently from relatively cheap raw materials, secondly, it contains the electron cloud on the aromatic ring or, the electro negative atoms such as nitrogen and oxygen in the relatively long chain compounds. In the present study, (NE)‐2‐methyl‐N‐(thiophen‐2‐ylmethylidene) aniline(T) was synthesized and its inhibiting action on the corrosion of mild steel in 1 M hydrochloric acid was examined by different corrosion methods, such as weight loss, potentiodynamic polarization and electrochemical impedance spectroscopy (EIS). The experimental results suggest that this compound is an efficient corrosion inhibitor and the inhibition efficiency increases with the increase in inhibitor concentration. Adsorption of this compound on mild steel surface obeys Langmuir’s isotherm. Correlation between quantum chemical calculations and inhibition efficiency of the investigated compound is discussed using the Density Functional Theory method (DFT).

Keywords: mild steel, Schiff base, inhibition, corrosion, HCl, quantum chemical

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Authors: N. Chahmana, I. Zerroual

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The aim of our work is the contribution to the improvement of the performances of the positive plate of the lead acid battery. For that, we synthesized two varieties of PbO2 used in industry, alpha and beta PbO2 by electrochemical way starting from the not formed industrial plates. We studied the kinetics of reduction of the alpha varieties and PbO2 beta on electrode with microcavity in sulphuric medium. The electrochemical study of the powders of α and β-PbO2 was made by cyclic voltamperometry with sweeping of potential by using a traditional assembly with three electrodes. Values of the coefficient of diffusion of the proton in α and β-PbO2 are respectively equal to 0.498*10-8cm2 /s and 0.793*10-8 cm2 /s. During the cycling of the two varieties of PbO2, we obtain a clear increase in the capacity.

Keywords: lead accumulator, α and β - PbO2, synthesis, kinetics, cyclic voltametry, coefficient of diffusion

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Authors: N. Ammouchi

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We have studied the effect of milling time on the structural and hyperfine properties of Ni45Al45Fe10 compound elaborated by mechanical alloying. The elaboration was performed by using the planetary ball mill at different milling times. The as milled powders were characterized by X-ray diffraction (XRD) and Mӧssbauer spectroscopy. From XRD diffraction spectra, we show that the β NiAl(Fe) was completely formed after 24 h of milling time. When the milling time increases, the lattice parameter increases, whereas the grain size decreases to a few nanometres and the mean level of microstrains increases. The analysis of Mӧssbauer spectra indicates that, in addition to a ferromagnetic phase, α-Fe, a paramagnetic disordered phase Ni Al (Fe) solid solution is observed after 2h and only this phase is present after 12h.

Keywords: NiAlFe, nanostructured powders, X-ray diffraction, Mӧssbauer spectroscopy

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Authors: William L. Whitehouse, Louisa H. Y. Lo, Andrew B. Kinghorn, Simon C. C. Shiu, Julian. A. Tanner

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C-reactive protein (CRP) is an acute-phase reactant and sensitive indicator for sepsis and other life-threatening pathologies, including systemic inflammatory response syndrome (SIRS). Currently, clinical turn-around times for established CRP detection methods take between 30 minutes to hours or even days from centralized laboratories. Here, we report the development of an electrochemical biosensor using redox probe-tagged DNA aptamers functionalized onto cheap, commercially available screen-printed electrodes. Binding-induced conformational switching of the CRP-targeting aptamer induces a specific and selective signal-ON event, which enables single-step and reagentless detection of CRP in as little as 1 minute. The aptasensor dynamic range spans 5-1000nM (R=0.97) or 5-500nM (R=0.99) in 50% diluted human serum, with a LOD of 3nM, corresponding to 2-orders of magnitude sensitivity under the clinically relevant cut-off for CRP. The sensor is stable for up to one week and can be reused numerous times, as judged from repeated real-time dosing and dose-response assays. By decoupling binding events from the signal induction mechanism, structure-switching electrochemical aptamer-based sensors (SS-EABs) provide considerable advantages over their adsorption-based counterparts. Our work expands on the retinue of such sensors reported in the literature and is the first instance of an SS-EAB for reagentless CRP detection. We hope this study can inspire further investigations into the suitability of SS-EABs for diagnostics, which will aid translational R&D toward fully realized devices aimed at point-of-care applications or for use more broadly by the public.

Keywords: structure-switching, C-reactive protein, electrochemical, biosensor, aptasensor.

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Authors: Tomilola J. Ajayi, Moses Ollengo, Lukas le Roux, Michael N. Pillay, Richard J. Staples, Shannon M. Biros Werner E. van Zyl

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The formation, characterization, and dye-sensitized solar cell application of nickel(II), zinc(II) and cadmium(II) ferrocenyl dithiophosphonate complexes were investigated. The multidentate monoanionic ligand [S₂PFc(OH)]¯ (L1) was synthesized from the reaction between ferrocenyl Lawesson’s reagent, [FcP(=S)μ-S]₂ (FcLR), (Fc = ferrocenyl) and water. Ligand L1 could potentially coordinate to metal centers through the S, S’ and O donor atoms. The reaction between metal salt precursors and L1 produced a Ni(II) complex of the type [Ni{S₂P(Fc)(OH)}₂] (1) (molar ratio 1:2), a tetranickel (II) complex of the type [Ni₂{S₂OP(Fc)}₂]₂ (2) (molar ratio (1:1), as well as a Zn(II) complex [Zn{S₂P(Fc)(OH)}₂]₂ (3), and a Cd(II) complex [Cd{S₂P(Fc)(OH)}₂]₂ (4). Complexes 1-4 were characterized by 1H and 31P NMR and FT-IR, and complexes 1 and 2 were additionally analysed by X-Ray crystallography. After co-sensitization, the DSSCs were characterized using UV-Vis, cyclic voltammetry, electrochemical impedance spectroscopy, and photovoltaic measurements (I-V curves). Overall finding shows that co-sensitization of our compounds with ruthenium dye N719 resulted in a better overall solar conversion efficiency than only pure N719 dye under the same experimental conditions. In conclusion, we report the first examples of dye-sensitized solar cells (DSSCs) co-sensitized with ferrocenyl dithiophosphonate complexes.

Keywords: dithiophosphonate, dye sensitized solar cell, co-sensitization, solar efficiency

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Authors: Wasi Khan, Suboohi Shervani, Swaleha Naseem, Mohd. Shoeb, J. A. Khan, B. R. Singh, A. H. Naqvi

Abstract:

We have successfully synthesized ZnO/TiO2 nanocomposite using a two-step solochemical synthesis method. The influence of annealing temperature on microstructural, optical, anticandidal, photocatalytic activities and dielectric properties were investigated. X-ray diffraction (XRD) and scanning electron microscopy (SEM) show the formation of nanocomposite and uniform surface morphology of all samples. The UV-Vis spectra indicate decrease in band gap energy with increase in annealing temperature. The anticandidal activity of ZnO/TiO2 nanocomposite was evaluated against MDR C. albicans 077. The in-vitro killing assay revealed that the ZnO/TiO2 nanocomposite efficiently inhibit the growth of the C. albicans 077. The nanocomposite also exhibited the photocatalytic activity for the degradation of methyl orange as a function of time at 465 nm wavelength. The electrical behaviour of composite has been studied over a wide range of frequencies at room temperature using complex impedance spectroscopy. The dielectric constants, dielectric loss and ac conductivity (σac) were studied as the function of frequency, which have been explained by ‘Maxwell Wagner Model’. The data reveals that the dielectric constant and loss (tanδ) exhibit the normal dielectric behavior and decreases with the increase in frequency.

Keywords: ZnO/TiO2 nanocomposites, SEM, photocatalytic activity, dielectric properties

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Authors: Sarah Fahad Alajmi, Tamer Ezzat Youssef

Abstract:

Here, we report a simple method for the direct conversion of 6-Nitro-1H-indole into N-substituted indoles via electrochemical dehydrogenative reaction with halogenated reagents under strongly basic conditions through N–R bond formation. The N-protected indoles have been prepared under moderate and scalable electrolytic conditions. The conduct of the reactions was performed in a simple divided cell under constant current without oxidizing reagents or transition-metal catalysts. The synthesized products have been characterized via UV/Vis spectrophotometry, 1H-NMR, and FTIR spectroscopy. A possible reaction mechanism is discussed based on the N-protective products. This methodology could be applied to the synthesis of various biologically active N-substituted indole derivatives.

Keywords: green chemistry, 1H-indole, heteroaromatic, organic electrosynthesis

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Authors: Maria Sofia Palagonia, Doriano Brogioli, Fabio La Mantia

Abstract:

In the last decade, lithium has become an important raw material in various sectors, in particular for rechargeable batteries. Its production is expected to grow more and more in the future, especially for mobile energy storage and electromobility. Until now it is mostly produced by the evaporation of water from salt lakes, which led to a huge water consumption, a large amount of waste produced and a strong environmental impact. A new, clean and faster electrochemical technique to recover lithium has been recently proposed: electrochemical ion pumping. It consists in capturing lithium ions from a feed solution by intercalation in a lithium-selective material, followed by releasing them into a recovery solution; both steps are driven by the passage of a current. In this work, a new configuration of the electrochemical cell is presented, used to study and optimize the process of the intercalation of lithium ions through the hydrodynamic condition. Lithium Manganese Oxide (LiMn₂O₄) was used as a cathode to intercalate lithium ions selectively during the reduction, while Nickel Hexacyano Ferrate (NiHCF), used as an anode, releases positive ion. The effect of hydrodynamics on the process has been studied by conducting the experiments at various fluxes of the electrolyte through the electrodes, in terms of charge circulated through the cell, captured lithium per unit mass of material and overvoltage. The result shows that flowing the electrolyte inside the cell improves the lithium capture, in particular at low lithium concentration. Indeed, in Atacama feed solution, at 40 mM of lithium, the amount of lithium captured does not increase considerably with the flux of the electrolyte. Instead, when the concentration of the lithium ions is 5 mM, the amount of captured lithium in a single capture cycle increases by increasing the flux, thus leading to the conclusion that the slowest step in the process is the transport of the lithium ion in the liquid phase. Furthermore, an influence of the concentration of other cations in solution on the process performance was observed. In particular, the capturing of the lithium using a different concentration of NaCl together with 5 mM of LiCl was performed, and the results show that the presence of NaCl limits the amount of the captured lithium. Further studies can be performed in order to understand why the full capacity of the material is not reached at the highest flow rate. This is probably due to the porous structure of the material since the liquid phase is likely not affected by the convection flow inside the pores. This work proves that electrochemical ion pumping, with a suitable hydrodynamic design, enables the recovery of lithium from feed solutions at the lower concentration than the sources that are currently exploited, down to 1 mM.

Keywords: desalination battery, electrochemical ion pumping, hydrodynamic, lithium

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Authors: Chetna Tyagi. G. B. V. S. Lakshmi, Ambuj Tripathi, D. K. Avasthi

Abstract:

Graphene oxide provides a good host matrix for preparing nanocomposites due to the different functional groups attached to its edges and planes. Being biocompatible, it is used in therapeutic applications. As enzyme-based biosensor requires complicated enzyme purification procedure, high fabrication cost and special storage conditions, we need enzyme-less biosensors for use even in a harsh environment like high temperature, varying pH, etc. In this work, we have prepared both enzyme-based and enzyme-less graphene oxide-based biosensors for glucose detection using glucose-oxidase as enzyme and gold nanoparticles, respectively. These samples were characterized using X-ray diffraction, UV-visible spectroscopy, scanning electron microscopy, and transmission electron microscopy to confirm the successful synthesis of the working electrodes. Electrochemical measurements were performed for both the working electrodes using a 3-electrode electrochemical cell. Cyclic voltammetry curves showed the homogeneous transfer of electron on the electrodes in the scan range between -0.2V to 0.6V. The sensing measurements were performed using differential pulse voltammetry for the glucose concentration varying from 0.01 mM to 20 mM, and sensing was improved towards glucose in the presence of gold nanoparticles. Gold nanoparticles in graphene oxide nanocomposite played an important role in sensing glucose in the absence of enzyme, glucose oxidase, as evident from these measurements. The selectivity was tested by measuring the current response of the working electrode towards glucose in the presence of the other common interfering agents like cholesterol, ascorbic acid, citric acid, and urea. The enzyme-less working electrode also showed storage stability for up to 15 weeks, making it a suitable glucose biosensor.

Keywords: electrochemical, enzyme-less, glucose, gold nanoparticles, graphene oxide, nanocomposite

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Authors: Arezoo Assarian, Reza Javaherdashti

Abstract:

Microbiologically influenced corrosion (MIC) is an electrochemical process that can affect both metals and non-metals. The cost of MIC can amount to 40% of the cost of corrosion. MIC is enhanced via factors such as but not limited to the presence of certain bacteria and archaea as well as mechanisms such as external electron transfer. There are five methods by which electrochemical corrosion, including MIC, can be prevented, of which coatings are an effective method due to blinding anode, cathode and, electrolyte from each other. Conventional ordinary coatings may themselves become nutrient sources for the bacteria and therefore show low efficiency in dealing with MIC. Recently our works on polyaspartic coating (DTM) have shown promising results, therefore nominating DTM as the most appropriate coating material to manage both MIC and general electrochemical corrosion very efficiently. Nanosilver particles are known for their antimicrobial properties that make them of desirable distractive impacts on any germs. This coating will be formulated based on Nanosilver phosphate and copper II oxide in the resin network and co-reactant. The nanoparticles are light and heat-sensitive agents. The method which is used to keep nanoparticles in the film coating is the encapsulation of active ingredients. By this method, it will prevent incompatibility between different particles. For producing microcapsules, the interfacial cross-linking method will be used. This is achieved by adding an active ingredient to an aqueous solution of the cross-linkable polymer. In this paper, we will first explain the role of coating materials in controlling and preventing electrochemical corrosion. We will explain MIC and some of its fundamental principles, such as bacteria establishment (biofilm) and the role they play in enhancing corrosion via mechanisms such as the establishment of differential aeration cells. Later we will explain features of DTM coatings that highly contribute to preventing biofilm formation and thus microbial corrosion.

Keywords: biofilm, corrosion, microbiologically influenced corrosion(MIC), nanosilver particles, polyaspartic coating (DTM)

Procedia PDF Downloads 167