Search results for: electrochemical characterization

Authors: Parvin Samadi Pakchin, Reza Saber, Hossein Ghanbari, Yadollah Omidi

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Ovarian cancer is one of the leading cause of mortality among the gynecological malignancies, and it remains the one of the most prevalent cancer in females worldwide. Tumor markers are biochemical molecules in blood or tissues which can indicates cancers occurrence in the human body. So, the sensitive and specific detection of cancer markers typically recruited for diagnosing and evaluating cancers. Recently extensive research efforts are underway to achieve a simple, inexpensive and accurate device for detection of cancer biomarkers. Compared with conventional immunoassay techniques, electrochemical immunosensors are of great interest, because they are specific, simple, inexpensive, easy to handling and miniaturization. Moreover, in the past decade nanotechnology has played a crucial role in the development of biosensors. In this study, a signal-off electrochemical immunosensor for the detection of CA125 antigen has been developed using chitosan-gold nanoparticles (CS-AuNP) and multi-wall carbon nanotubes (MWCNT) composites. Toluidine blue (TB) is used as redox probe which is immobilized on the electrode surface. CS-AuNP is synthesized by a simple one step method that HAuCl4 is reduced by NH2 groups of chitosan. The CS-AuNP-MWCNT modified electrode has shown excellent electrochemical performance compared with bare Au electrode. MWCNTs and AuNPs increased electrochemical conductivity and accelerate electrons transfer between solution and electrode surface while excessive amine groups on chitosan lead to the effective loading of the biological material (CA125 antibody) and TB on the electrode surface. The electrochemical, immobilization and sensing properties CS-AuNP-MWCNT-TB modified electrodes are characterized by cyclic voltammetry, electrochemical impedance spectroscopy, differential pulse voltammetry and square wave voltammetry with Fe(CN)63−/4−as an electrochemical redox indicator.

Keywords: signal-off electrochemical biosensor, CA125, ovarian cancer, chitosan-gold nanoparticles

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Authors: T. Abohalkuma, J. Telegdi

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Preparation, characterization, and application of self-assembled monolayers (SAM) formed by fluorophosphonic and undecenyl phosphonic acids on carbon steel surfaces as anticorrosive nanocoatings were demonstrated. The anticorrosive efficacy of these SAM layers was followed by atomic force microscopy, as the change in the surface morphology caused by layer deposition and corrosion processes was monitored. The corrosion process was determined by electrochemical potentiodynamic polarization, whereas the surface wettability of the carbon steel samples was tested with the use of static and dynamic contact angle measurements. Results showed that both chemicals produced good protection against corrosion as they performed as anodic inhibitors, especially with increasing the time of layer formation, which results in a more compact molecular film. According to the atomic force microscope (AFM) images, the fluoro-phosphonic acid self-assembled molecular layer can control the general as well as the pitting corrosion, but the SAM layers of the undecenyl-phosphonic acid cannot inhibit the pitting corrosion. The AFM and the contact angle measurements confirmed the results achieved by electrochemical measurements.

Keywords: nanolayers, corrosion, phosphonic acids, coatings

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Authors: Tien S. H. Pham, Peter J. Mahon, Aimin Yu

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The detection of drug molecules by voltammetry has attracted great interest over the past years. However, many drug molecules exhibit poor electrochemical signals at common electrodes which result in low sensitivity in detection. An efficient way to overcome this problem is to modify electrodes with functional materials. Since discovered in 2004, graphene (or reduced graphene oxide) has emerged as one of the most studied two-dimensional carbon materials in condensed matter physics, electrochemistry, and so on due to its exceptional physicochemical properties. Additionally, the continuous development of technology has opened the new window for the successful fabrications of many novel graphene-based nanomaterials to serve in electrochemical analysis. This research aims to synthesize and characterize gold nanoparticle coated beta-cyclodextrin functionalized reduced graphene oxide (Au NP–β-CD–RGO) nanocomposites with highly conductive and strongly electro-catalytic properties as well as excellent supramolecular recognition abilities for the modification of electrodes. The electrochemical responses of ciprofloxacin at the as-prepared nanocomposite modified electrode was effectively amplified was much higher in comparison with that at the bare electrode. The linear concentration range was from 0.01 to 120 µM, with a detection limit of 2.7 nM using differential pulse voltammetry. Thus, Au NP–β-CD–RGO nanocomposite has great potential as an ideal material to construct sensitive sensors for the electrochemical determination of ciprofloxacin or similar antibacterial drugs in the future based on its excellent stability, selectivity, and reproducibility.

Keywords: Au nanoparticles, β-CD, ciprofloxacin, electrochemical determination, graphene based nanomaterials

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Authors: Alaeddine Kaouka

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The properties and characterization of Ti-6Al-4V alloys with different contents of Mo were investigated. Microstructure characterization and hardness are considered. The alloy structure was characterized by X-ray diffraction, SEM and optical microscopy. The results showed that the addition of Mo stabilized the β-phase in the treated solution condition. The Mo element added to titanium alloys changes the lattice parameters of phases. Microstructural observations indicate an obvious reduction in the prior grain size. The hardness has increased with the increase in β-phase stability, while Young’s modulus and ductility have decreased.

Keywords: characterization, mechanical properties, molybdenum, titanium alloy

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Authors: A. Asselah, A. Khalfi, M. A.Toumi, A.Tazerouti

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The study of the corrosion inhibition of a standard carbon steel "API 5L grade X70" by two biodegradable anionic surfactants derived from fatty acids by photo sulfochlorination, called sodium lauryl methyl ester sulfonates and sodium palmityl methyl ester sulfonates was carried. A solution at 2.5 g/l NaCl saturated with carbon dioxide is used as a corrosive medium. The gravimetric and electrochemical technics (stationary and transient) were used in order to quantify the rate of corrosion and to evaluate the electrochemical inhibition efficiency, thus the nature of the mode of action of the inhibitor, in addition to a surface characterization by scanning electron microscopy (MEB) coupled to energy dispersive X-ray spectroscopy (EDX). The variation of the concentration and the temperature were examined, and the mode of adsorption of these inhibitors on the surface of the metal was established by assigning it the appropriate isotherm and determining the corresponding thermodynamic parameters. The MEB-EDX allowed the visualization of good adhesion of the protective film formed by the surfactants to the surface of the steel. The corrosion inhibition was evaluated at around 93% for sodium lauryl methyl ester sulfonate surfactant at 20 ppm and 87.2% at 50 ppm for sodium palmityl methyl ester sulfonate surfactant.

Keywords: carbon steel, oilfield, corrosion, anionic surfactants

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Authors: Jinjoo Jung, Hayeon Won, Doyeong Jeong, Do Hyung Kim

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We present the electrochemical and electrochromic performance of the novel crystalline tungsten oxide and tungsten-molybdenum oxide nanostructures synthesized by utilizing solvo-thermal method with hexacarbonyl tungsten, hexacarbonyl molybdenum, and ethyl alcohol. The morphology and phase of the prepared products were highly dependent on the synthesis conditions such as synthesis and annealing temperature, synthesis time, and precursor ratio. The tungsten oxide nanostructures (TCNs) have urchin-like or spherical nanostructure with different phase of W18O49 and WO3. The morphology of tungsten-molybdenum oxide nanostructures (TMONs) is basically similar to that of TCNs. However, the morphology and phase of TMONs are more diverse and are strongly dependent on the composition ratios of W/Mo in the precursor. The electrochemical properties depending on their morphologies and phases of TCNs and TMONs are compared using cyclic voltammetry and galvanostatic charge/discharge tests. The relationship between the electrochromic performance and phase structures/morphologies of nanostructured TCNs and TMONs are systematically investigated.

Keywords: electrochemical, electrochromic, tungsten oxide, tungsten-molybdenum oxide

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Authors: Abdi Djamila, Haffar Hichem

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The poly methylene bleu (PMB) has been successfully electro deposited on fluorine doped tin oxide (FTO) conducting glass as substrate. Its optical, electrical and photoelectrochemical characterizations have been carried out in order to show the performances of such polymer. The deposited film shows a good electric conductivity which is well confirmed by the low gap value determinated optically by UV–vis spectroscopy. Like all polymers the PMB presents an absorption difference in the visible range function of the polarization potential, it is expressed by the strong conjugation at oxidized state but is weakened with leucoform formation at reduced state. The electrochemical analysis of the films permit to show the cyclic voltamperogram with the anodic oxidation and cathodic reduction states of the polymer and to locate the corresponding energy levels HOMO and LUMO of this later. The electrochemical impedance spectroscopy permit to see the conductive character of such film and to calculate important parameters as Rtc and CPE. The study of the photoelectro activity of our polymer shows that under exposure to intermittent light source this later exhibit important photocurrents which enables it to be used in photo organic ells.

Keywords: polymethylene blue, electropolymerization, homo-lumo, photocurrents

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Authors: Dhanashree Aole, V. Hariharan, Swati Surushe

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Corrosion can cause serious and expensive damage to the automobile components. Various proven techniques for controlling and preventing corrosion depend on the specific material to be protected. Electrochemical Impedance Spectroscopy (EIS) and salt spray tests are commonly used to assess the corrosion degradation mechanism of coatings on metallic surfaces. While, the only test which monitors the corrosion rate in real time is known as Linear Polarisation Resistance (LPR). In this study, electrochemical tests (EIS & LPR) and spray test are reviewed to assess the corrosion resistance and durability of different coatings. The main objective of this study is to correlate the test results obtained using linear polarization resistance (LPR) and Electrochemical Impedance Spectroscopy (EIS) with the results obtained using standard salt spray test. Another objective of this work is to evaluate the performance of various coating systems- CED, Epoxy, Powder coating, Autophoretic, and Zn-trivalent coating for vehicle underbody application. The corrosion resistance coating are assessed. From this study, a promising correlation between different corrosion testing techniques is noted. The most profound observation is that electrochemical tests gives quick estimation of corrosion resistance and can detect the degradation of coatings well before visible signs of damage appear. Furthermore, the corrosion resistances and salt spray life of the coatings investigated were found to be according to the order as follows- CED> powder coating > Autophoretic > epoxy coating > Zn- Trivalent plating.

Keywords: Linear Polarization Resistance (LPR), Electrochemical Impedance Spectroscopy (EIS), salt spray test, sacrificial and barrier coatings

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Authors: Sujit Kumar Guchhait, Subir Paul

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One of the major research areas is to find an alternative source of energy to fulfill the energy crisis and environmental problems. The Fuel cell is such kind of energy producing unit. Use of fuel cell to produce renewable energy for commercial purpose is limited by the high cost of Pt based electrode material. Development of high energetic, as well as inexpensive fuel cell electrode materials, is needs of hour to produce clean energy using derive bio-fuel. In this present investigation, inexpensive Cu-Ni-CeO2 electrode material has been synthesized by using pulse current. The surface morphology of the electrode materials is controlled by several deposition parameters to increase the rate of electrochemical oxidation of alcoholic fuel, ethanol. The electrochemical characterization of the developed material was done by Cyclic Voltammetry (CV) and Chronoamperometry (CA) and Electrochemical Impedance Spectroscopy test. It is interesting to find that both these materials have shown high electrocatalytic properties in terms of high exchange current density (I0), low polarization resistance (Rp) and low impedance. It is seen that the addition of CeO2 to Ni-Cu has outperformed Pt as far as high electrocatalytic properties are concerned. The exchange current density on the Cu-Ni-CeO2 electrode surface for ethanol oxidation is about eight times higher than the same on the Pt surface with much lower polarization resistance than the later. The surface morphology of the electrode materials has been revealed by Field Effect Scanning Electron Microscope (FESEM). It is seen that grains are narrow and subspherical with 3D surface containing pores in between two elongated grains. XRD study exhibits the presence of Ni and CeO2 on the Cu surface.

Keywords: electro-catalyst, alcoholic fuel, cyclic voltammetry, potentiodynamic polarization, EIS, XRD, SEM

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Authors: Uc-Cayetano E. G., Ake-Uh O. E., Villanueva-Mena I. E., Ordonez L. C.

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Carbon nanotubes (CNTs) and other graphitic nanostructures are materials with extraordinary physical, physicochemical and electrochemical properties which are being aggressively investigated for a variety of sensing applications. Thus, sensing of biological molecules such as proteins, DNA, glucose and other enzymes using either single wall or multiwall carbon nanotubes (MWCNTs) has been widely reported. Despite the current progress in this area, the electrochemical response of CNTs used in a variety of sensing arrangements still needs to be improved. An alternative towards the enhancement of this CNTs' electrochemical response is to chemically (or physically) modify its surface. The influence of the decoration with iron oxide nanoparticles in different types of MWCNTs on the amperometric sensing of glucose, urea, and cholesterol in solution is investigated. Commercial MWCNTs were oxidized in acid media and subsequently decorated with iron oxide nanoparticles; finally, the enzymes glucose oxidase, urease, and cholesterol oxidase are chemically immobilized to oxidized and decorated MWCNTs for glucose, urease, and cholesterol electrochemical sensing. The results of the electrochemical characterizations consistently show that the presence of iron oxide nanoparticles decorating the surface of MWCNTs enhance the amperometric response and the sensitivity to increments in glucose, urease, and cholesterol concentration when compared to non-decorated MWCNTs.

Keywords: WCNTs, enzymes, oxidation, decoration

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Authors: Ahmed A. Al-Amiery, Yasmin K. Al-Majedy, Abdul Amir H. Kadhum, Abu Bakar Mohamad

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The efficiency of synthesized thiosemicarbazone namely 2-(1,5-dimethyl-4-(2-methylbenzylidene)amino)-2-phenyl-1H-pyrazol-3(2H)-ylidene) hydrazinecarbothioamide investigated as corrosion inhibitor of mild steel in 1N H2SO4 using electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization (PD) in addition of scanning electron microscopy (SEM). The results showed that this inhibitor behaved as a good corrosion inhibitor even at low concentration with a mean efficiency of 93%. Polarization technique and EIS were tested in different concentrations reveal that this compound is adsorbed on the mild steel, therefore blocking the active sites and the adsorption follows the Langmuir adsorption isotherm model. SEM shows that mild steel surface is nearly perfect for mild steel which was immersed in a solution of H2SO4 with corrosion inhibitor.

Keywords: corrosion inhibitor, thiosemicarbazide, electrochemical impedance, electrochemical impedance spectroscopy

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Authors: S. Habibi, T. E. Guarcia, A. Megueni, A. Ziadi, L. Aminallah, A. S. Bouchikhi

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The characterization of the microstructure of Dual Phase steel in various low-carbon, with a yield stress between 400 and 900 MPa were conducted .In order to assess the mechanical properties of steel, we examined the influence of their chemical compositions interictal and heat treatments (austenite + ferrite area) on their micro structures. In this work, we have taken a number of commercial DP steels, micro structurally characterized and used the conventional tensile testing of these steels for mechanical characterization.

Keywords: characterization, construction in civil engineering, micro structure, tensile DP steel

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Authors: A. K. Singh, Chhotu Ram

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The present work relates to the corrosivity of distillery effluent and corrosion performance of mild steel and stainless steels SS304L, SS316L, and 2205. The report presents the results and conclusions drawn on the basis of (i) electrochemical polarization tests performed in distillery effluent and laboratory prepared solutions having composition similar to that of the effluent (ii) the surface examination by scanning electron microscope (SEM) of the corroded steel samples. It is observed that pH and presence of chloride, phosphate, calcium, nitrite and nitrate in distillery effluent enhance corrosion, whereas presence of sulphate and potassium inhibits corrosion. Among the materials tested, mild steel is observed to experience maximum corrosion followed by stainless steels SS304L, SS316L, and 2205.

Keywords: corrosion, distillery effluent, electrochemical polarization, steel

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Authors: Eyob Belew Abebe

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Nickel-rich layered oxide cathode materials having a Ni content of ≥ 90% have great potential for use in next-generation lithium-ion batteries (LIBs), due to their high energy densities and relatively low cost. They suffer, however, from poor cycling performance and rate capability, significantly hampering their widespread applicability. In this study we synthesized a Ni-rich precursor through a co-precipitation method and added different amounts of Li-excess on the precursors using a solid-state method to obtain sintered Li1+x(Ni0.9Co0.05Mn0.05)1–xO2 (denoted as L1+x-NCM; x = 0.00, 0.02, 0.04, 0.06, and 0.08) transition metal (TM) oxide cathode materials. The L1+x-NCM cathode having a Li-excess of 4% exhibited a discharge capacity of ca. 216.17 mAh g–1 at 2.7–4.3 V, 0.1C and retained 95.7% of its initial discharge capacity (ca. 181.39 mAh g–1) after 100 cycles of 1C charge/discharge which is the best performance as compared with stoichiometric Li1+x(Ni0.9Co0.05Mn0.05)1-xO2 (i.e. x=0, Li:TM = 1:1). Furthermore, a high-rate capability of ca. 162.92 mAh g–1 at a rate of 10C, led to the 4% Li-excess optimizing the electrochemical performance, relative to the other Li-excess samples. Ex/in-situ X-ray diffraction, scanning electron microscopy, and X-ray photoelectron spectroscopy revealed that the 4% Li-excess in the Ni-rich NCM90 cathode material: (i). decreased the Li+/Ni2+ disorder by increasing the content of Ni3+ in the TM slab, (ii). increased the crystallinity, and (iii). accelerated Li+ ion transport by widening the Li-slab. Furthermore, electrochemical impedance spectroscopy and cyclic voltammetry confirmed that the appropriate Li-excess lowered the electrochemical impedance and improved the reversibility of the electrochemical reaction. Therefore, our results revealed that NCM90 cathode materials featuring an optimal Li-excess are potential candidates for use in next-generation Li-ion batteries.

Keywords: LiNi₀.₉Co₀.₀₉Mn₀.₀₉O₂, li-excess, cation mixing, structure change, cycle stability, electrochemical properties

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Authors: Yu-Jen Shih, Juan-Zhang Lou

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Nitrogenous compounds, such as NH4+/NH3 and NO3-, have become important contaminants in water resources. Excessive concentration of NH3 leads to eutrophication, which poses a threat to aquatic organisms in the environment. Electrochemical oxidation emerged as a promising water treatment technology, offering advantages such as simplicity, small-scale operation, and minimal reliance on additional chemicals. In this study, a nickel-based metal-organic framework (Ni-MOF) was synthesized using 2-amino terephthalic acid (BDC-NH2) and nickel nitrate. The Ni-MOF was further carbonized as derived nickel oxide and nitrogen-carbon composite, Ni/NiOx/NC. The nickel oxide within the 2D porous carbon texture served as active sites for ammonia oxidation. Results of characterization showed that the Ni-MOF was a hexagonal and flaky nanoparticle. With increasing carbonization temperature, the nickel ions in the organic framework re-crystallized as NiO clusters on the surfaces of the 2D carbon. The electrochemical surface area of Ni/NiOx/NC significantly increased as to improve the efficiency of ammonia oxidation. The phase transition of Ni(OH)2⇌NiOOH at around +0.8 V was the primary mediator of electron transfer. Batch electrolysis was conducted under constant current and constant potential modes. The electrolysis parameters included pyrolysis temperatures, pH, current density, initial feed concentration, and electrode potential. The constant current batch experiments indicated that via carbonization at 800 °C, Ni/NiOx/NC(800) was able to decrease the ammonium nitrogen of 50 mg-N/L to below 1 ppm within 4 hours at a current density of 3 mA/cm2 and pH 11 with negligible oxygenated nitrogen formation. The constant potential experiments confirmed that N2 nitrogen selectivity was enhanced up to 90% at +0.8 V.

Keywords: electrochemical oxidation, nickel oxyhydroxide, metal-organic framework, ammonium, nitrate

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Authors: H. M. Mohammad, A. Martin, N. Brown, N. Hodson, P. Hill, E. Roberts

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Graphite intercalation compound (GIC) has been demonstrated to be a useful, low capacity and rapid adsorbent for the removal of organic micropollutants from water. The high electrical conductivity and low capacity of the material lends itself to electrochemical regeneration. Following electrochemical regeneration, equilibrium loading under similar conditions is reported to exceed that achieved by the fresh adsorbent. This behavior is reported in terms of the regeneration efficiency being greater than 100%. In this work, surface analysis techniques are employed to investigate the material in three states: ‘Fresh’, ‘Loaded’ and ‘Regenerated’. ‘Fresh’ GIC is shown to exhibit a hydrogen and oxygen rich surface layer approximately 150 nm thick. ‘Loaded’ GIC shows a similar but slightly thicker surface layer (approximately 370 nm thick) and significant enhancement in the hydrogen and oxygen abundance extending beyond 600 nm from the surface. 'Regenerated’ GIC shows an oxygen rich layer, slightly thicker than the fresh case at approximately 220 nm while showing a very much lower hydrogen enrichment at the surface. Results demonstrate that while the electrochemical regeneration effectively removes the phenol model pollutant, it also oxidizes the exposed carbon surface. These results may have a significant impact on the estimation of adsorbent life.

Keywords: graphite, adsorbent, electrochemical, regeneration, phenol

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Authors: O. Guellati, A. Harat, F. Djefaflia, N. Habib, A. Nait-Merzoug, J. El Haskouri, D. Momodu, N. Manyala, D. Bégin, M. Guerioune

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We report a facile and low-cost free-template synthesis method was used to synthesize mesoporous smart multifunctional nanohybrids based on Graphene/PANI nanofibers micro/nanostructures with very interesting physic-chemical properties and faradic electrochemical behavior of these products was investigated. These nanohybrid products have been characterized quantitatively and qualitatively using different techniques, such as XRD / FTIR, Raman, XPS spectroscopy, Field Emission SEM and High-Resolution TEM microscopy, BET textural analysis, electrochemical measurements (CV, CD, EIS). Moreover, the electrochemical measurements performed in a 6 M KOH aqueous electrolyte depicted excellent electrochemical performance ascribed to the optimized composition of hydroxides et PANI nanofibers. An exceptionally notable specific capacitance between 800  and 2000 F. g-1 was obtained at 5  mV. s-1 scan rate for these synthesized products depends on the optimized growth conditions. We found much better nanohybrids by reinforcing hydroxides or conduction polymer nanofibers with carbonaceous nanomaterials depicting their potential as suitable materials for energy storage devices.

Keywords: nanohybrid materials, conducting polymers, carbonaceous nanomaterials, supercapacitors, energy storage

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Authors: Yongkui Cui, Fengping Wang, Hailei Zhao, Muhammad Zubair Iqbal, Ziya Wang, Yan Li, Pengpeng LV

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The novel 3D SnO cabbages self-assembled by nanosheets were successfully synthesized via template-free hydrothermal growth method under facile conditions.The XRD results manifest that the as-prepared SnO is tetragonal phase. The TEM and HRTEM results show that the cabbage nanosheets are polycrystalline structure consisted of considerable single-crystalline nanoparticles. Two typical Raman modes A1g=210 and Eg=112 cm-1 of SnO are observed by Raman spectroscopy. Moreover, galvanostatic cycling tests has been performed using the SnO cabbages as anode material of lithium ion battery and the electrochemical results suggest that the synthesized SnO cabbage structures are a promising anode material for lithium ion batteries.

Keywords: electrochemical property, hydrothermal synthesis, lithium ion battery, stannous oxide

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Authors: Hany M. Abd El-Lateef

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Two novel Schiff bases, 5-bromo-2-[(E)-(pyridin-3-ylimino) methyl] phenol (HBSAP) and 5-bromo-2-[(E)-(quinolin-8-ylimino) methyl] phenol (HBSAQ) have been synthesized. They have been characterized by elemental analysis and spectroscopic techniques (UV–Vis, IR and NMR). Moreover, the molecular structure of HBSAP and HBSAQ compounds are determined by single crystal X-ray diffraction technique. The inhibition activity of HBSAP and HBSAQ for carbon steel in 3.5 %NaCl+0.1 M HCl for both short and long immersion time, at different temperatures (20-50 ºC), was investigated using electrochemistry and surface characterization. The potentiodynamic polarization shows that the inhibitors molecule is more adsorbed on the cathodic sites. Its efficiency increases with increasing inhibitor concentrations (92.8 % at the optimal concentration of 10-3 M for HBSAQ). Adsorption of the inhibitors on the carbon steel surface was found to obey Langmuir’s adsorption isotherm with physical/chemical nature of the adsorption, as it is shown also by scanning electron microscopy. Further, the electronic structural calculations using quantum chemical methods were found to be in a good agreement with the results of the experimental studies.

Keywords: carbon steel, Schiff bases, corrosion inhibition, SEM, electrochemical techniques

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Authors: H. Abu-Ali, A. Nabok, T. Smith

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Aptamers are single-strand of DNA or RNA nucleotides sequence which is designed in vitro using selection process known as SELEX (systematic evolution of ligands by exponential enrichment) were developed for the selective detection of many toxic materials. In this work, we have developed an electrochemical biosensor for highly selective and sensitive detection of Hg2+ and Pb2+ using a specific aptamer probe (SAP) labelled with ferrocene (or methylene blue) in (5′) end and the thiol group at its (3′) termini, respectively. The SAP has a specific coil structure that matching with G-G for Pb2+ and T-T for Hg2+ interaction binding nucleotides ions, respectively. Aptamers were immobilized onto surface of screen-printed gold electrodes via SH groups; then the cyclic voltammograms were recorded in binding buffer with the addition of the above metal salts in different concentrations. The resulted values of anode current increase upon binding heavy metal ions to aptamers and analyte due to the presence of electrochemically active probe, i.e. ferrocene or methylene blue group. The correlation between the anodic current values and the concentrations of Hg2+ and Pb2+ ions has been established in this work. To the best of our knowledge, this is the first example of using a specific DNA aptamers for electrochemical detection of heavy metals. Each increase in concentration of 0.1 μM results in an increase in the anode current value by simple DC electrochemical test i.e (Cyclic Voltammetry), thus providing an easy way of determining Hg2+ and Pb2+concentration.

Keywords: aptamer, based, biosensor, DNA, electrochemical, highly, specific

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Authors: Tareg Omar Mansour, Khaled Omar Elhaji

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Model solutions of pentanol in the salt water of various concentrations were subjected to electrochemical oxidation using a dimensionally stable anode (DSA) and a platinised titanium cathode. The removal of pentanol was analysed over time using gas chromatography (GC) and by monitoring the total organic carbon (TOC) concentration of the reaction mixture. It was found that the removal of pentanol occurred more efficiently at higher salinities and higher applied electrical current values. When using a salt concentration of 20,000 ppm and an applied current of 100 mA there was a decrease in concentration of pentanol of 15 %. When the salt concentration and applied current were increased to 58,000 ppm and 500 mA respectively, the decrease in concentration was improved to 64 %.

Keywords: dimensionally stable anode (DSA), total organic hydrocarbon (TOC), gas chromatography mass spectrometry (GCMS), electrochemical oxidation

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Authors: Ana P. R. N. Barroso, Maurício N. Kleinberg, Frederico R. Silva, Rodrigo F. Guimarães, Marcelo M. V. Parente, Walney S. Araújo

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The fight against accelerated wear of the equipment used in the oil and gas sector is a challenge for minimizing maintenance costs. Corrosion being one of the main agents of equipment deterioration, we seek alternative materials that exhibit improved corrosion resistance at low cost of production. This study aims to evaluate the corrosion behavior of experimental alloys containing 15% and 17% of chromium (Cr) and 5% of molybdenum (Mo) in comparison with an AISI 444 commercial alloy. Microstructural analyzes were performed on samples of the alloys before and after the electrochemical tests. Two samples of each solubilized alloy were also taken for analysis of the corrosion behavior by testing potentiodynamic polarization (PP) and Electrochemical Impedance Spectroscopy (EIS) with immersion time of 24 hours in electrolytic solution with acidic character. The graphics obtained through electrochemical tests of PP and EIS indicated that among the experimental alloys, the alloy with higher chromium content (17%) had a higher corrosion resistance, confirming the beneficial effect of adding chromium. When comparing the experimental alloys with the AISI 444 commercial alloy, it is observed that the AISI 444 commercial alloy showed superior corrosion resistance to that of the experimental alloys for both assays, PP and EIS. The microstructural analyzes performed after the PP and EIS tests confirmed the results previously described. These results suggest that the addition of these levels of molybdenum did not favor the electrochemical behavior of experimental ferritic alloys for the electrolytic medium studied.

Keywords: corrosion, molybdenum, electrochemical tests, experimental alloys

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Authors: Zakaria Ahmed, Khaled Charradi, Sherif M. A. S. Keshk, Radhouane Chtourou

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Sulfonated poly ether ether ketone (SPEEK) with a low sulfonation degree was blended using nanofiller Layered Double Hydroxide (LDH, Mg2AlCl) /sepiolite nanostructured material as additive to use as an electrolyte membrane for fuel cell application. Characterization assessments, i.e., mechanical stability, thermal gravimetric analysis, ion exchange capability, swelling properties, water uptake capacities, electrochemical impedance spectroscopy analysis, and Fourier transform infrared spectroscopy (FTIR) of the composite membranes were conducted. The presence of LDH/sepiolite nanoarchitecture material within SPEEK was found to have the highest water retention and proton conductivity value at high temperature rather than LDH/SPEEK and pristine SPEEK membranes.

Keywords: SPEEK, sepiolite clay, LDH clay, proton exchange membrane

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Authors: Asmae Tafraouti, Yasmina Layouni

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The fabrication of cylindrical Tungsten micro-tools with a high aspect ratio is a real challenge because of several constraints that come into during their manufacture. In this paper, we will describe the process used to fabricate these micro-tools. It consists of using electrochemical etching. We will also present the optimal protocol that makes it possible to fabricate micro-tools with a high aspect ratio in a reproducible way. Next, we will show the limit of the experimental parameters chosen to manufacture micro-tools from a wire with an initial diameter of Φ_0=250µm. The protocol used allows obtaining an average diameter of Φ=88µm ±1 µm over a length of L=3.5mm.

Keywords: drop-off effect, electrochemical etching, micro-electrical discharge machining, tungsten micro-tools

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Authors: Seval Yilmaz, Filiz Bayrakci Karel, Ali Savas Koparal

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Textile products produced by leather have been indispensable for human consumption. Various chemicals are used to enhance the durability of end-products in the processing of leather products. The wastewaters from the leather industry which contain these chemicals exhibit toxic effects on the receiving environment and threaten the natural ecosystem. In this study, leather industry wastewater (LIW), which has high loads of contaminants, was treated using advanced treatment techniques instead of conventional methods. During the experiments, the performance of electrochemical methods was investigated. During the electrochemical experiments, the performance of batch electrooxidation (EO) using boron-doped diamond (BDD) electrodes with monopolar configuration for removal of chemical oxygen demand (COD) from LIW were investigated. The influences of electrolysis time, current density (which varies as 5 mA/cm², 10 mA/cm², 20 mA/cm², 30 mA/cm², 50 mA/cm²) and initial pH (which varies as 3,80 (natural pH of LIW), 7, 9) on removal efficiency were investigated in a batch stirred cell to determine the best treatment conditions. The current density applied to the electrochemical reactors is directly proportional to the consumption of electric energy, so electrical energy consumption was monitored during the experiment. The best experimental conditions obtained in electrochemical studies were as follows: electrolysis time = 60 min, current density = 30.0 mA/cm², pH 7. Using these parameters, 53.59% COD removal rates for LIW was achieved and total energy consumption was obtained as 13.03 kWh/m³. It is concluded that electrooxidation process constitutes a plausible and developable method for the treatment of LIW.

Keywords: BDD electrodes, COD removal, electrochemical treatment, leather industry wastewater

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Authors: Mohamed Benaicha, Mahdi Allam

Abstract:

A new two stage electrochemical process as a safe, large area and low processing cost technique for the production of semi-conducting CuInSe2 (CIS) thin films is studied. CuIn precursors were first potentiostatically electrodeposited onto molybdenum substrates from an acidic thiocyanate electrolyte. In a second stage, the prepared metallic CuIn layers were used as substrate in the selenium electrochemical deposition system and subjected to a thermal treatment in vacuum atmosphere, to eliminate binary phase formation by reaction of the Cu2-x Se and InxSey selenides, leading to the formation of CuInSe2 thin film. Electrochemical selenization from aqueous electrolyte is introduced as an alternative to toxic and hazardous H2Se or Se vapor phase selenization used in physical techniques. In this study, the influence of film deposition parameters such as bath composition, temperature and potential on film properties was studied. The electrochemical, morphological, structural and compositional properties of electrodeposited thin films were characterized using various techniques. Results of Cyclic and Stripping-Cyclic Voltammetry (CV, SCV), Scanning Electron Microscopy (SEM) and Energy Dispersive X-Ray microanalysis (EDX) investigations revealed good reproducibility and homogeneity of the film composition. Thereby optimal technological parameters for the electrochemical production of CuIn, Se as precursors for CuInSe2 thin layers are determined.

Keywords: photovoltaic, CIGS, copper alloys, electrodeposition, thin films

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Authors: Megha, Diksha, Seema Rani, Balwinder Kaur, Harminder Kaur

Abstract:

Fe₃O₄@SiO₂@SB functionalized magnetic nanoparticles were synthesized and used to detect heavy metal ions such as Pb²⁺, Hg²⁺, and Cd²⁺ in water. The formation of Fe₃O₄@SiO₂@SB nanocatalyst was confirmed by XRD, SEM, TEM, and IR. The simultaneous determination of analyte cations was carried out using square wave anodic stripping voltammetry (SWASV). Investigation and optimisation were done to study how experimental variables affected the performance of the modified magnetic electrode. Pb²⁺, Hg²⁺, and Cd²⁺ were successfully detected using the designed sensor in the presence of various possibly interfering ions. The recovery rate was found to be 97.5% for Pb²⁺, 96.2% for Hg²⁺, 103.5% for Cd²⁺. The electrochemical sensor was also employed to determine the presence of heavy metal ions in drinking water samples, which are well below the World Health Organization (WHO) guidelines.

Keywords: magnetic nanoparticles, heavy metal ions, electrochemical sensor, environmental water samples

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Authors: A. N. Fouda

Abstract:

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

Abstract:

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: Snehal L. Kadam, Shriniwas B. Kulkarni

Abstract:

Flexible electrode material with high surface area and good electrochemical properties is the current trend captivating the researchers across globe for application in the next generation energy storage field. In the present work, crumpled sheet like reduced graphene oxide grown on carbon cloth by the hydrothermal method with a series of different deposition temperatures at fixed time. The influence of the deposition temperature on the structural, morphological, optical and supercapacitive properties of the electrode material was investigated by XRD, RAMAN, XPS, TEM, FE-SEM, UV-VISIBLE and electrochemical characterization techniques.The results show that the hydrothermally synthesized reduced graphene oxide on carbon cloth has sheet like mesoporous structure. The reduced graphene oxide material at 160°C exhibits the best supercapacitor performance, with a specific capacitance of 443 F/g at scan rate 5mV/sec. Moreover, stability studies show 97% capacitance retention over 1000 CV cycles. This result shows that hydrothermally synthesized RGO on carbon cloth is the potential electrode material and would be used in the next-generation wearable energy storage systems. The detailed analysis and results will be presented at the conference.

Keywords: graphene oxide, reduced graphene oxide, carbon cloth, deposition temperature, supercapacitor

Procedia PDF Downloads 163