Search results for: electrochemical

Authors: Navpreet Kaur, Himkusha Thakur, Nirmal Prabhakar

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One of the most publicized and controversial issue in crop production is the use of agrichemicals- also known as pesticides. This is evident in many reports that Organophosphate (OP) insecticides, among the broad range of pesticides are mainly involved in acute and chronic poisoning cases. Therefore, detection of OPs is very necessary for health protection, food and environmental safety. In our study, a nanocomposite of poly (3,4 ethylenedioxythiophene) (PEDOT) and multi-walled carbon nanotubes (MWCNTs) has been deposited electrochemically onto the surface of fluorine doped tin oxide sheets (FTO) for the analysis of malathion OP. The -COOH functionalization of MWCNTs has been done for the covalent binding with amino groups of AChE enzyme. The use of PEDOT-MWCNT films exhibited an excellent conductivity, enables fast transfer kinetics and provided a favourable biocompatible microenvironment for AChE, for the significant malathion OP detection. The prepared PEDOT-MWCNT/FTO and AChE/PEDOT-MWCNT/FTO nano-biosensors were characterized by Fourier transform infrared spectrometry (FTIR), Field emission-scanning electron microscopy (FE-SEM) and electrochemical studies. Electrochemical studies were done using Cyclic Voltammetry (CV) or Differential Pulse Voltammetry (DPV) and Electrochemical Impedance Spectroscopy (EIS). Various optimization studies were done for different parameters including pH (7.5), AChE concentration (50 mU), substrate concentration (0.3 mM) and inhibition time (10 min). The detection limit for malathion OP was calculated to be 1 fM within the linear range 1 fM to 1 µM. The activity of inhibited AChE enzyme was restored to 98% of its original value by 2-pyridine aldoxime methiodide (2-PAM) (5 mM) treatment for 11 min. The oxime 2-PAM is able to remove malathion from the active site of AChE by means of trans-esterification reaction. The storage stability and reusability of the prepared nano-biosensor is observed to be 30 days and seven times, respectively. The application of the developed nano-biosensor has also been evaluated for spiked lettuce sample. Recoveries of malathion from the spiked lettuce sample ranged between 96-98%. The low detection limit obtained by the developed nano-biosensor made them reliable, sensitive and a low cost process.

Keywords: PEDOT-MWCNT, malathion, organophosphates, acetylcholinesterase, nano-biosensor, oxime (2-PAM)

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Authors: Maxim Panov, Evgenia Khairullina, Sergey Ermakov, Oleg Gundobin, Vladimir Kochemirovsky

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The continuous in situ laser-induced catalysis proceeding via generation and growth of nano-sized copper particles was discussed. Also, the simple and lost-cost method for manufacturing of microstructural copper electrodes was proposed. The electrochemical properties of these electrodes were studied by cyclic voltammetry and impedance spectroscopy. The surface of the deposited copper structures (electrodes) was investigated by X-ray photoelectron spectroscopy and atomic force microscopy. These microstructures are highly conductive and porous with a dispersion of pore size ranging from 50 nm to 50 μm. An analytical response of the fabricated copper electrode is 30 times higher than those observed for a pure bulk copper with similar geometric parameters. A study of sensory characteristics for hydrogen peroxide determination showed that the value of Faraday current at the fabricated copper electrode is 2-2.5 orders of magnitude higher than for etalon one.

Keywords: laser-induced deposition, electrochemical electrodes, non-enzymatic sensors, copper

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Authors: Anju Joshi, C. N. Tharamani

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Diabetes is one of the leading cause of death at present and remains an important concern as the prevalence of the disease is increasing at an alarming rate. Therefore, it is crucial to diagnose the accurate levels of glucose for developing an efficient therapeutic for diabetes. Due to the availability of convenient and compact self-testing, continuous monitoring of glucose is feasible nowadays. Enzyme based electrochemical sensing of glucose is quite popular because of its high selectivity but suffers from drawbacks like complicated purification and immobilization procedures, denaturation, high cost, and low sensitivity due to indirect electron transfer. Hence, designing a robust enzyme free platform using transition metal oxides remains crucial for the efficient and sensitive determination of glucose. In the present work, manganese doped nickel oxide nanoparticles (Mn-NiO) has been synthesized onto the surface of multiwalled carbon nanotubes using a simple microwave assisted approach for non-enzymatic electrochemical sensing of glucose. The morphology and structure of the synthesized nanostructures were characterized using scanning electron microscopy (SEM) and X-Ray diffraction (XRD). We demonstrate that the synthesized nanostructures show enormous potential for electrocatalytic oxidation of glucose with high sensitivity and selectivity. Cyclic voltammetry and square wave voltammetry studies suggest superior sensitivity and selectivity of Mn-NiO decorated carbon nanotubes towards the non-enzymatic determination of glucose. A linear response between the peak current and the concentration of glucose has been found to be in the concentration range of 0.01 μM- 10000 μM which suggests the potential efficacy of Mn-NiO decorated carbon nanotubes for sensitive determination of glucose.

Keywords: diabetes, glucose, Mn-NiO decorated carbon nanotubes, non-enzymatic

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Authors: M. Mominul Haque, Danny KY. Wong

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In this paper, we will demonstrate the feasibility of selectively removing the azo dye, Acid Red 1, in the presence of a second dye, Indigo Carmine, at conducting polypyrrole films. A long-term goal of this work is to develop an efficient and effective electrochemical treatment of textile effluents that does not yield any toxic by-products. Specifically, pyrrole was initially electrochemically oxidised in the presence of Acid Red 1 to prepare an Acid Red 1-entrapped polypyrrole film. Next, the Acid Red 1 entrapped film was electrochemically reduced to expel the dye from the film. The film was then ready for use in removing the dye in an Acid Red 1 solution. The entrapment efficiency of the film was then studied by spectroscopically determining the change in the absorbance of the dye solution. These experiments were repeated using Indigo Carmine or a mixture of Acid Red 1 and Indigo Carmine, in place of Acid Red 1. Therefore, this has given rise to an environmentally friendly treatment method for textile effluents. In our work, we have also studied the characteristics of Acid Red 1- and Indigo Carmine-entrapped polypyrrole films by scanning electron microscopy, X-ray diffraction and Fourier transfer infrared spectroscopy.

Keywords: azo dye, electrochemical treatment, polypyrrole, Acid Red 1

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Authors: Desplanches Maxime

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Accurate estimation of the remaining useful life of lithium-ion batteries for electronic devices is crucial. Data-driven methodologies encounter challenges related to data volume and acquisition protocols, particularly in capturing a comprehensive range of aging indicators. To address these limitations, we propose a hybrid approach that integrates an electrochemical model with state-of-the-art data analysis techniques, yielding a comprehensive database. Our methodology involves infusing an aging phenomenon into a Newman model, leading to the creation of an extensive database capturing various aging states based on non-destructive parameters. This database serves as a robust foundation for subsequent analysis. Leveraging advanced data analysis techniques, notably principal component analysis and t-Distributed Stochastic Neighbor Embedding, we extract pivotal information from the data. This information is harnessed to construct a regression function using either random forest or support vector machine algorithms. The resulting predictor demonstrates a 5% error margin in estimating remaining battery life, providing actionable insights for optimizing usage. Furthermore, the database was built from the Newman model calibrated for aging and performance using data from a European project called Teesmat. The model was then initialized numerous times with different aging values, for instance, with varying thicknesses of SEI (Solid Electrolyte Interphase). This comprehensive approach ensures a thorough exploration of battery aging dynamics, enhancing the accuracy and reliability of our predictive model. Of particular importance is our reliance on the database generated through the integration of the electrochemical model. This database serves as a crucial asset in advancing our understanding of aging states. Beyond its capability for precise remaining life predictions, this database-driven approach offers valuable insights for optimizing battery usage and adapting the predictor to various scenarios. This underscores the practical significance of our method in facilitating better decision-making regarding lithium-ion battery management.

Keywords: Li-ion battery, aging, diagnostics, data analysis, prediction, machine learning, electrochemical model, regression

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Authors: H. Farokhi, A. Bahadoran

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This paper is focused on the absorbance and magnetic properties of a novel nanocomposite based on conducting polymer, carbon black and barium hexaferrite in epoxy resin on the E-glass fibre substrate. The highly conductive nanocomposite was provided by in-situ polymerization of aniline in the presence of carbon black (C) and barium hexaferrite (BaFe12O19) as electromagnetic absorbance material. The structure, morphology, and magnetic properties of samples were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). SEM images showed the uniformly coated PAni on the surface of carbon black and barium hexaferrite. XRD peaks also verified the presence of carbon black and barium hexaferrite in the nanocomposite. The microwave characteristics determined from the magnetic and dielectric properties of the elastomeric composites obtained from scattering data by fitting the samples in a waveguide, where measured in the frequency in X-band frequency range, the range of 8 to 12 GHz. The reflection losses were evaluated to be less than −5dB over the whole X-band frequency (8–12 GHz) for the thickness of 1.4mm.

Keywords: conductive polymer, magnetic materials, capacitance, electrochemical cell

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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: Majid Farsadrouh Rashti, Parisa Jahani, Amir Shafiee, Mehrdad Mofidi

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The dihydroxybenzene isomers, hydroquinone (HQ), catechol (CC) and resorcinol (RS) have been widely recognized as important environmental pollutants due to their toxicity and low degradability in the ecological environment. Speciation of HQ, CC and RS is very important for environmental analysis because they co-exist of these isomers in environmental samples and are too difficult to degrade as an environmental contaminant with high toxicity. There are many analytical methods have been reported for detecting these isomers, such as spectrophotometry, fluorescence, High-performance liquid chromatography (HPLC) and electrochemical methods. These methods have attractive advantages such as simple and fast response, low maintenance costs, wide linear analysis range, high efficiency, excellent selectivity and high sensitivity. A novel modified glassy carbon electrode (GCE) with Pd@ Cu/CNTs core−shell nanowires for the simultaneous determination of hydroquinone (HQ), catechol (CC) and resorcinol (RS) is described. A detailed investigation by field emission scanning electron microscopy and electrochemistry was performed in order to elucidate the preparation process and properties of the GCE/ Pd/CuNWs-CNTs. The electrochemical response characteristic of the modified GPE/LFOR toward HQ, CC and RS were investigated by cyclic voltammetry, differential pulse voltammetry (DPV) and Chronoamperometry. Under optimum conditions, the calibrations curves were linear up to 228 µM for each with detection limits of 0.4, 0.6 and 0.8 µM for HQ, CC and RS, respectively. The diffusion coefficient for the oxidation of HQ, CC and RS at the modified electrode was calculated as 6.5×10⁻⁵, 1.6 ×10⁻⁵ and 8.5 ×10⁻⁵ cm² s⁻¹, respectively. DPV was used for the simultaneous determination of HQ, CC and RS at the modified electrode and the relative standard deviations were 2.1%, 1.9% and 1.7% for HQ, CC and RS, respectively. Moreover, GCE/Pd/CuNWs-CNTs was successfully used for determination of HQ, CC and RS in real samples.

Keywords: dihydroxybenzene isomers, galvanized copper nanowires, electrochemical sensor, Palladium, speciation

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Authors: Olfat E. El-Azabawy, Enas M. Attia, Nadia Shawky, Amira M. Hypa

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In this work, an attempt is made to study the effects of orange peel extract (OPE) as an environment-friendly corrosion inhibitor for carbon steel (CS) within a formation water solution (FW). The study was performed in different concentrations (0.5-2.5% (v/v)) of peel extracts at ambient temperatures (25oC) and (2.5% (v/v)) at temperature range (25- 55 oC) by weight loss measurements, open circuit potential, potentiodynamic polarization and electrochemical impedance. The inhibition efficiency was calculated from all measurements and confirmed by energy-dispersive X-ray spectroscopy (EDS). Inhibition was found to increase with increasing inhibitors concentration and decrease with increasing temperature. It was seen that IE% is about 92.84% in the presence of 2.5% (v/v) of orange peel inhibitor by using weight loss method. The adsorption process was of physical type and obey Langmuir adsorption isotherm. Also, adsorption, as well as the inhibition process, followed first-order kinetics at all concentrations.

Keywords: eco-friendly corrosion inhibitor, OPE, oilfield water, electrochemical impedance

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Authors: Ingy N. Bkrey, Ahmed A. Moniem

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We succeeded to produce a high performance and flexible graphene/Manganese dioxide (G/MnO2) electrode coated on flexible polyethylene terephthalate (PET) substrate. The graphene film is initially synthesized by drop-casting the graphene oxide (GO) solution on the PET substrate, followed by simultaneous reduction and patterning of the dried film using carbon dioxide (CO2) laser beam with power of 1.8 W. Potentiostatic Anodic Deposition method was used to deposit thin film of MnO2 with different loading mass 10 – 50 and 100 μg.cm-2 on the pre-prepared graphene film. The electrodes were fully characterized in terms of structure, morphology, and electrochemical performance. A maximum specific capacitance of 973 F.g-1 was attributed when depositing 50 μg.cm-2 MnO2 on the laser reduced graphene oxide rGO (or G/50MnO2) and over 92% of its initial capacitance was retained after 1000 cycles. The good electrochemical performance and long-term cycling stability make our proposed approach a promising candidate in the supercapacitor applications.

Keywords: electrode deposition, flexible, graphene oxide, graphene, high power CO2 Laser, MnO2

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Authors: Monika Sogani, Zainab Syed, Adrian C. Fisher

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Pollution of estrogenic compounds has caught the attention of researchers as the slight increase of estrogens in the water bodies has a significant impact on the aquatic system. They belong to a class of endocrine disrupting compounds (EDCs) and are able to mimic hormones or interfere with the action of endogenous hormones. The microbial electrochemical remediation system (MERS) is employed here for exploiting an electrophototrophic bacterium for evaluating the capacity of biodegradation of ethinylestradiol hormone (EE2) under anaerobic conditions with power generation. MERS using electro-phototrophic bacterium offers a tailored solution of wastewater treatment in a developing country like India which has a huge solar potential. It is a clean energy generating technology as they require only sunlight, water, nutrients, and carbon dioxide to operate. Its main feature that makes it superior over other technologies is that the main fuel for this MERS is sunlight which is indefinitely present. When grown in light with organic compounds, these photosynthetic bacteria generate ATP by cyclic photophosphorylation and use carbon compounds to make cell biomass (photoheterotrophic growth). These cells showed EE2 degradation and were able to generate hydrogen as part of the process of nitrogen fixation. The two designs of MERS were studied, and a maximum of 88.45% decrease in EE2 was seen in a total period of 14 days in the better design. This research provides a better insight into microbial electricity generation and self-sustaining wastewater treatment facilities. Such new models of waste treatment aiming waste to energy generation needs to be followed and implemented for building a resource efficient and sustainable economy.

Keywords: endocrine disrupting compounds, ethinylestradiol, microbial electrochemical remediation systems, wastewater treatment

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Authors: Abdur Rahim, Lauro Tatsuo Kubota, Yoshitaka Gushikem

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Carbon ceramic mesoporous SiO2/50wt%C (SBET= 170 m2g-1), where C is graphite, was prepared by the sol gel method. Scanning electron microscopy images and the respective element mapping showed that, within the magnification used, no phase segregation was detectable. It presented the electric conductivities of 0.49 S cm-1. This material was used to support cobalt phthalocyanine, prepared in situ, to assure a homogeneous dispersion of the electro active complex in the pores of the matrix. The surface density of cobalt phthalocyanine, on the matrix surfaces was 0.015 mol cm-2. Pressed disk, made with SiO2/50wt%C/CoPc, was used to fabricate an electrode and tested as sensors for nitrite determination by electro chemical technique. A linear response range between 0.039 and 0.42 mmol l−1,and correlation coefficient r=0.9996 was obtained. The electrode was chemically very stable and presented very high sensitivity for this analyte, with a limit of detection, LOD = 1.087 x 10-6 mol L-1.

Keywords: SiO2/C/CoPc, sol-gel method, electrochemical sensor, nitrite oxidation, carbon ceramic material, cobalt phthalocyanine

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Authors: Amandeep Singh Oberoi, John Andrews, Alan L. Chaffee, Lachlan Ciddor

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Electrochemical storage of hydrogen in activated carbon electrodes as part of a reversible fuel cell offers a potentially attractive option for storing surplus electrical energy from inherently variable solar and wind energy resources. Such a system – which we have called a proton flow battery – promises to have roundtrip energy efficiency comparable to lithium ion batteries, while having higher gravimetric and volumetric energy densities. Activated carbons with high internal surface area, high pore volume, light weight and easy availability have attracted considerable research interest as a solid-state hydrogen storage medium. This paper compares the physical characteristics and hydrogen storage capacities of four activated carbon electrodes made by different methods from brown coal. The fabrication methods for these samples are explained. Their proton conductivity was measured using electrochemical impedance spectroscopy, and their hydrogen storage capacity by galvanostatic charging and discharging in a three-electrode electrolytic cell with 1 mol sulphuric acid as electrolyte. The highest hydrogen storage capacity obtained was 1.29 wt%, which compares favourably with metal hydrides used in commercially available solid-state hydrogen storages. The hydrogen storage capacity of the samples increased monotonically with increasing BET surface area (calculated from CO2 adsorption method). The results point the way towards selecting high-performing electrodes for proton flow batteries that the competitiveness of this energy storage technology.

Keywords: activated carbon, electrochemical hydrogen storage, proton flow battery, proton conductivity

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Authors: David Polcari, Samuel C. Perry, Loredano Pollegioni, Matthias Geissler, Janine Mauzeroll

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ᴅ-serine acts as an endogenous co-agonist for N-methyl-ᴅ-aspartate receptors in neuronal synapses. This makes it a key component in the development and function of a healthy brain, especially given its role in several neurodegenerative diseases such as Alzheimer’s disease and dementia. Despite such clear research motivations, the primary site and mechanism of ᴅ-serine release is still currently unclear. For this reason, we are developing a biosensor for the detection of ᴅ-serine utilizing a microelectrode in combination with a ᴅ-amino acid oxidase enzyme, which produces stoichiometric quantities of hydrogen peroxide in response to ᴅ-serine. For the fabrication of a biosensor with good selectivity, we use a permselective poly(meta-phenylenediamine) film to ensure only the target molecule is reacted, according to the size exclusion principle. In this work, we investigated the effect of the electrodeposition conditions used on the biosensor’s response time and selectivity. Careful optimization of the fabrication process allowed for enhanced biosensor response time. This allowed for the real time sensing of ᴅ-serine in a bulk solution, and also provided in means to map the efflux of ᴅ-serine in real time. This was done using scanning electrochemical microscopy (SECM) with the optimized biosensor to measure localized release of ᴅ-serine from an agar filled glass capillary sealed in an epoxy puck, which acted as a model system. The SECM area scan simultaneously provided information regarding the rate of ᴅ-serine flux from the model substrate, as well as the size of the substrate itself. This SECM methodology, which provides high spatial and temporal resolution, could be useful to investigate the primary site and mechanism of ᴅ-serine release in other biological samples.

Keywords: ᴅ-serine, enzymatic biosensor, microelectrode, scanning electrochemical microscopy

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Authors: M.S. Ashraf, Raja Rizwan Hussain, A. M. Alhozaimy

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The effect of supplementary cementitious materials (SCMs) with concrete pore solution on the protective properties of the oxide films that form on reinforcing steel bars has been experimentally investigated using electrochemical impedance spectroscopy (EIS) and Tafel Scan. The tests were conducted on oxide films grown in saturated calcium hydroxide solutions that included different representative amounts of NaOH and KOH. In addition to that, commonly used supplementary cementitious materials (natural pozzolan and fly ash) were also added. The results of electrochemical tests show that supplementary cementitious materials do have an effect on the protective properties of the passive oxide film. In particular, natural pozzolans has been shown to have a highly positive influence on the film quality. Fly ash also increases the protective qualities of the passive film.

Keywords: supplementary cementitious materials (SCMs), passive film, EIS, Tafel scan, rebar, concrete, simulated concrete pore solution (SPS)

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Authors: Yu. Mateyshina, A. Ulihin, N. Uvarov

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Supercapacitors are one of the most promising devices for energy storage applications as they can provide higher power density than batteries and higher energy density than conventional dielectric capacitors. Carbon materials with various microtextures are considered as main candidates for supercapacitors in terms of high surface area, interconnected pore structure, controlled pore size, high electrical conductivity and environmental friendliness. The specific capacitance (C) of the electrode material of the Electrochemical Double Layer Capacitors (EDLC) is known to depend on the specific surface area (Ss) and the pore structure. Activated carbons are most commonly used in supercapacitors because of their high surface area (Ss ≥ 1000 m2/g), good adhesion to electrolytes and low cost. In this work, electrochemical properties of new microporous and mesoporous carbon electrode materials were studied. The aim of the work was to investigate the relationship between the specific capacitance and specific surface area in a series of materials prepared from different organic precursors.. As supporting matrixes different carbon samples with Ss = 100-2000 m2/g were used. The materials were modified by treatment in acids (H2SO4, HNO3, acetic acid) in order to enable surface hydrophilicity. Then nanoparticles of transition metal oxides (for example NiO) were deposited on the carbon surfaces using methods of salts impregnation, mechanical treatment in ball mills and the precursors decomposition. The electrochemical characteristics of electrode hybrid materials were investigated in a symmetrical two-electrode cell using an impedance spectroscopy, voltammetry in both potentiodynamic and galvanostatic modes. It was shown that the value of C for the materials under study strongly depended on the preparation method of the electrode and the type of electrolyte (1 M H2SO4, 6 M KOH, 1 M LiClO4 in acetonitryl). Specific capacity may be increased by the introduction of nanoparticles from 50-100 F/g for initial carbon materials to 150-300 F/g for nanocomposites which may be used in supercapacitors. The work is supported by the по SC-14.604.21.0013.

Keywords: supercapacitors, carbon electrode, mesoporous carbon, electrochemistry

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Authors: Gaurav Bhanjana, Ganga Ram Chaudhary, Sandeep Kumar, Neeraj Dilbaghi

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Main sources of endocrine disrupting compounds in the ecosystem are hormones, pesticides, phthalates, flame retardants, dioxins, personal-care products, coplanar polychlorinated biphenyls (PCBs), bisphenol A, and parabens. These endocrine disrupting compounds are responsible for learning disabilities, brain development problems, deformations of the body, cancer, reproductive abnormalities in females and decreased sperm count in human males. Although discharge of these chemical compounds into the environment cannot be stopped, yet their amount can be retarded through proper evaluation and detection techniques. The available techniques for determination of these endocrine disrupting compounds mainly include high performance liquid chromatography (HPLC), mass spectroscopy (MS) and gas chromatography-mass spectrometry (GC–MS). These techniques are accurate and reliable but have certain limitations like need of skilled personnel, time consuming, interference and requirement of pretreatment steps. Moreover, these techniques are laboratory bound and sample is required in large amount for analysis. In view of above facts, new methods for detection of endocrine disrupting compounds should be devised that promise high specificity, ultra sensitivity, cost effective, efficient and easy-to-operate procedure. Nowadays, electrochemical sensors/biosensors modified with nanomaterials are gaining high attention among researchers. Bioelement present in this system makes the developed sensors selective towards analyte of interest. Nanomaterials provide large surface area, high electron communication feature, enhanced catalytic activity and possibilities of chemical modifications. In most of the cases, nanomaterials also serve as an electron mediator or electrocatalyst for some analytes.

Keywords: electrochemical, endocrine disruptors, microscopy, nanoparticles, sensors

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Authors: A. Hamam, D. Oukil, A. Dib, L. Makhloufi

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The aim of this work is to synthesize modified Polypyrrole films (PPy) containing nanoparticles of copper oxides onto a non conducting cellulosic substrate. Firstly, the chemical polymerization of polypyrrole onto cellulosic substrate is carried out using FeCl3 as an oxidant and Pyrrole as monomer. Different parameters were optimized (monomer concentration, duration of the experiment, nature of supporting electrolyte, temperature, etc.) in order to obtain films with different thickness and different morphologies. Thickness and topography of different PPy deposits were estimated by a profilometer apparatus. The electrochemical reactivity of the obtained electrodes were tested by cyclic voltammetry technique (CV) and electrochemical impedance spectroscopy (EIS). Secondly, the modification of the PPy film surface by incorporation of copper oxide nanonoparticles is conducted by applying a galvanostatic procedure from CuCl2 solution. Surface characterization has been carried out using scanning microscope (SEM) coupled with energy dispersive X-ray analysis (EDX), Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The analysis showed the presence of the copper oxide nanoparticles (CuO) in the polymer films with dimensions less than 50 nm.

Keywords: polypyrrole, modified electrode, cellulosic substrate, copper oxide

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Authors: V. Pérez-Herranz, C. González-Buch, E. M. Ortega, S. Mestre

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In this work new macroporous Ni electrodes modified with Au nanoparticles for hydrogen production have been developed. The supporting macroporous Ni electrodes have been obtained by means of the electrodeposition at high current densities. Then, the Au nanoparticles were synthesized and added to the electrode surface. The electrocatalytic behaviour of the developed electrocatalysts was studied by means of pseudo-steady-state polarization curves, electrochemical impedance spectroscopy (EIS) and hydrogen discharge curves. The size of the Au synthetized nanoparticles shows a monomodal distribution, with a very sharp band between 10 and 50 nm. The characteristic parameters d10, d50 and d90 were 14, 20 and 31 nm respectively. From Tafel polarization data has been concluded that the Au nanoparticles improve the catalytic activity of the developed electrodes towards the HER respect to the macroporous Ni electrodes. EIS permits to obtain the electrochemically active area by means of the roughness factor value. All the developed electrodes show roughness factor values in the same order of magnitude. From the activation energy results it can be concluded that the Au nanoparticles improve the intrinsic catalytic activity of the macroporous Ni electrodes.

Keywords: Au nano particles, hydrogen evolution reaction, porous Ni electrodes, electrochemical impedance spectroscopy

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Authors: Jamal Hussain Al-Smail

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Hydrogen fuel cells (HFCs) are environmentally friendly, energy converter devices that convert the chemical energy of the reactants (oxygen and hydrogen) to electricity through electrochemical reactions. The level of the electricity production of HFCs mainly increases depending on the oxygen distribution in the HFC’s cathode gas diffusion layer (GDL). With a constant porosity of the GDL, the electrochemical reaction can have a great variation that reduces the cell’s productivity and stability. Our findings bring a methodology in finding porosity designs of the diffusion layer to improve the oxygen distribution such that it results in a stable oxygen-hydrogen reaction. We first introduce a mathematical model involving the mass and momentum transport equations, in which a porosity function of the GDL is incorporated as a control for the fluid flow. We then derive numerical methods for solving the mathematical model. In conclusion, we present our numerical results to show how to design the GDL porosity to result in a uniform oxygen distribution.

Keywords: fuel cells, material porosity design, mathematical modeling, porous media

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Authors: Ayomide A Sijuade, Nafiza Anjum

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The rising demand to meet the need for clean and sustainable energy solutions has led the market to create effective energy storage technologies. In this study, we look at the possibility of using a heterostructure made of polyaniline (PANI), titanium carbide (Ti₃C₂), and vanadium carbide (V₂C) for energy storage devices. V₂C is a two-dimensional transition metal carbide with remarkable mechanical and electrical conductivity. Ti₃C2 has solid thermal conductivity and mechanical strength. PANI, on the other hand, is a conducting polymer with customizable electrical characteristics and environmental stability. Layer-by-layer assembly creates the heterostructure of V₂C, Ti₃C₂, and PANI, allowing for precise film thickness and interface quality control. Structural and morphological characterization is carried out using X-ray diffraction, scanning electron microscopy, and atomic force microscopy. For energy storage applications, the heterostructure’s electrochemical performance is assessed. Electrochemical experiments, such as cyclic voltammetry and galvanostatic charge-discharge tests, examine the heterostructure’s charge storage capacity, cycle stability, and rate performance. Comparing the heterostructure to the individual components reveals better energy storage capabilities. V₂C, Ti₃C₂, and PANI synergize to increase specific capacitance, boost charge storage, and prolong cycling stability. The heterostructure’s unique arrangement of 2D materials and conducting polymers promotes effective ion diffusion and charge transfer processes, improving the effectiveness of energy storage. The heterostructure also exhibits remarkable electrochemical stability, which minimizes capacity loss after repeated cycling. The longevity and long-term dependability of energy storage systems depend on this quality. By examining the potential of V₂C, Ti₃C₂, and PANI heterostructures, the results of this study expand energy storage technology. These materials’ specialized integration and design show potential for use in hybrid energy storage systems, lithium-ion batteries, and supercapacitors. Overall, the development of high-performance energy storage devices utilizing V₂C, Ti₃C₂, and PANI heterostructures is clarified by this research, opening the door to the realization of effective, long-lasting, and eco-friendly energy storage solutions to satisfy the demands of the modern world.

Keywords: MXenes, energy storage materials, conductive polymers, composites

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Authors: Yunwei Zhang, Qiaochu Tang, Yao Zhang, Jiabin Wang, Ulrich Stimming, Alpha Lee

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Forecasting the state of health and remaining useful life of Li-ion batteries is an unsolved challenge that limits technologies such as consumer electronics and electric vehicles. Here we build an accurate battery forecasting system by combining electrochemical impedance spectroscopy (EIS) -- a real-time, non-invasive and information-rich measurement that is hitherto underused in battery diagnosis -- with Gaussian process machine learning. We collect over 20,000 EIS spectra of commercial Li-ion batteries at different states of health, states of charge and temperatures -- the largest dataset to our knowledge of its kind. Our Gaussian process model takes the entire spectrum as input, without further feature engineering, and automatically determines which spectral features predict degradation. Our model accurately predicts the remaining useful life, even without complete knowledge of past operating conditions of the battery. Our results demonstrate the value of EIS signals in battery management systems.

Keywords: battery degradation, machine learning method, electrochemical impedance spectroscopy, battery diagnosis

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Authors: B. D. Polat, Ö. Keleş

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Physical vapor deposition under conditions of an obliquely incident flux results in a film formation with an inclined columnar structure. These columns will be oriented toward the vapor source because of the self-shadowing effect, and they are homogenously distributed on the substrate surface because of the limited surface diffusion ability of ad-atoms when there is no additional substrate heating. In this work, the oblique angle electron beam evaporation technique is used to fabricate thin films containing inclined nanorods. The results demonstrate that depending on the thin film composition, the morphology of the nanorods changed as well. The galvanostatic analysis of these thin film anodes reveals that a composite CuSn nanorods having approximately 900mAhg-1 of initial discharge capacity, performs higher electrochemical performance compared to pure Sn nanorods containing anode material. The long cycle life and the advanced electrochemical properties of the nano-structured composite electrode might be attributed to its improved mechanical tolerance and enhanced electrical conductivity depending on the Cu presence in the nanorods.

Keywords: Cu-Sn thin film, oblique angle deposition, lithium ion batteries, anode

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Authors: Ashish Kumar Singh, Preeti Tiwari, Shubham Srivastava, Rajiv Prakash, Herman Terryn, Gopal Ji

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Corrosion inhibition potential of azo dyes namely Allura red (AR), Sunset Yellow (SY) and Amaranth (AN) have been investigated in 0.5 M H2SO4 solutions by electrochemical impedance spectroscopy (EIS), Tafel polarization curves, linear polarization curves, open circuit potential (ocp) curves, UV-Visible spectroscopy, Fourier Transform Infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) techniques. Amaranth dye is found to provide highest corrosion inhibition (90 %) against mild steel corrosion in sulfuric acid solutions among all the tested dyes; while SY and AR dye shows 80% and 78% corrosion inhibition efficiency respectively. The electrochemical measurements and surface morphology analysis reveal that molecular adsorption of dyes at metal acid interface is accountable for inhibition of mild steel corrosion in H2SO4 solutions. The adsorption behavior of dyes has been investigated by various isotherms models, which verifies that it is in accordance with Langmuir isotherm.

Keywords: mild steel, Azo dye, EIS, Langmuir isotherm

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Authors: Rovina Kobun, Shafiquzzaman Siddiquee

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A novel and simple electrochemical sensor for the determination of melamine was developed based on modified gold electrode (AuE) with chitosan (CHIT) nanocomposite membrane, zinc oxide nanoparticles (ZnONPs) and ionic liquids ([EMIM][Otf]) to enhance the potential current response of melamine. Cyclic voltammetry and differential pulse voltammetry were used to investigate the electrochemical behaviour between melamine and modified AuE in the presence of methylene blue as a redox indicator. The experimental results indicated that the interaction of melamine with CHIT/ZnONPs/([EMIM][Otf])/AuE were based on the strong interaction of hydrogen bonds. The morphological characterization of modified AuE was observed under scanning electron microscope. Under optimal conditions, the current signal was directly proportional to the melamine concentration ranging from 9.6 x 10-5 to 9.6 x 10-11 M, with a correlation coefficient of 0.9656. The detection limit was 9.6 x 10-12 M. Finally, the proposed method was successfully applied and displayed an excellent sensitivity in the determination of melamine in milk samples.

Keywords: melamine, gold electrode, zinc oxide nanoparticles, cyclic voltammetries, differential pulse voltammetries

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Authors: Pradakshina Sharma, Jagriti Narang

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Due to the critical significance in the early identification of infectious diseases, electrochemical sensors have garnered considerable interest. Here, we develop a detection platform for the chikungunya virus by rationally implementing the extremely high charge-transfer efficiency of a ternary nanocomposite of graphene oxide, silver, and gold (G/Ag/Au) (CHIKV). Because paper is an inexpensive substrate and can be produced in large quantities, the use of electrochemical paper analytical device (EPAD) origami further enhances the sensor's appealing qualities. A cost-effective platform for point-of-care diagnostics is provided by paper-based testing. These types of sensors are referred to as eco-designed analytical tools due to their efficient production, usage of the eco-friendly substrate, and potential to reduce waste management after measuring by incinerating the sensor. In this research, the paper's foldability property has been used to develop and create 3D multifaceted biosensors that can specifically detect the CHIKVX-ray diffraction, scanning electron microscopy, UV-vis spectroscopy, and transmission electron microscopy (TEM) were used to characterize the produced nanoparticles. In this work, aptamers are used since they are thought to be a unique and sensitive tool for use in rapid diagnostic methods. Cyclic voltammetry (CV) and linear sweep voltammetry (LSV), which were both validated with a potentiostat, were used to measure the analytical response of the biosensor. The target CHIKV antigen was hybridized with using the aptamer-modified electrode as a signal modulation platform, and its presence was determined by a decline in the current produced by its interaction with an anionic mediator, Methylene Blue (MB). Additionally, a detection limit of 1ng/ml and a broad linear range of 1ng/ml-10µg/ml for the CHIKV antigen were reported.

Keywords: biosensors, ePAD, arboviral infections, point of care

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Authors: Celine Bonnaud, Isabelle Billard, Nicolas Papaiconomou, Eric Chainet

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Thanks to their high magnetization and low mass, permanent magnets (NdFeB and SmCo) have quickly became essential for new energies (wind turbines, electrical vehicles…). They contain large quantities of neodymium, samarium and dysprosium, that have been recently classified as critical elements and that therefore need to be recycled. Electrochemical processes including electrodissolution followed by electrodeposition are an elegant and environmentally friendly solution for the recycling of such lanthanides contained in permanent magnets. However, electrochemistry of the lanthanides is a real challenge as their standard potentials are highly negative (around -2.5V vs ENH). Consequently, non-aqueous solvents are required. Ionic liquids (IL) are novel electrolytes exhibiting physico-chemical properties that fulfill many requirements of the sustainable chemistry principles, such as extremely low volatility and non-flammability. Furthermore, their chemical and electrochemical properties (solvation of metallic ions, large electrochemical windows, etc.) render them very attractive media to implement alternative and sustainable processes in view of integrated processes. All experiments that will be presented were carried out using butyl-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide. Linear sweep, cyclic voltammetry and potentiostatic electrochemical techniques were used. The reliability of electrochemical experiments, performed without glove box, for the classic three electrodes cell used in this study has been assessed. Deposits were obtained by chronoamperometry and were characterized by scanning electron microscopy and energy-dispersive X-ray spectroscopy. The IL cathodic behavior under different constraints (argon, nitrogen, oxygen atmosphere or water content) and using several electrode materials (Pt, Au, GC) shows that with argon gas flow and gold as a working electrode, the cathodic potential can reach the maximum value of -3V vs Fc+/Fc; thus allowing a possible reduction of lanthanides. On a gold working electrode, the reduction potential of samarium and neodymium was found to be -1.8V vs Fc+/Fc while that of dysprosium was -2.1V vs Fc+/Fc. The individual deposits obtained were found to be porous and presented some significant amounts of C, N, F, S and O atoms. Selective deposition of neodymium in presence of dysprosium was also studied and will be discussed. Next, metallic Sm, Nd and Dy electrodes were used in replacement of Au, which induced changes in the reduction potential values and the deposit structures of lanthanides. The individual corrosion potentials were also measured in order to determine the parameters influencing the electrodissolution of these metals. Finally, a full recycling process was investigated. Electrodissolution of a real permanent magnet sample was monitored kinetically. Then, the sequential electrodeposition of all lanthanides contained in the IL was investigated. Yields, quality of the deposits and consumption of chemicals will be discussed in depth, in view of the industrial feasibility of this process for real permanent magnets recycling.

Keywords: electrodeposition, electrodissolution, ionic liquids, lanthanides, rcycling

Procedia PDF Downloads 241

Authors: Yen-Ping Peng, Ku-Fan Chen, Ken-Lin Chang, Jian Sun

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In this study, palladium loaded titanium dioxide nanotube arrays (Pd/TNAs) was successfully synthesized by anodic oxidation etching method combined with microwave hydrothermal method, using tea or coffee as a green reductant. Pd/TNAs was employed as an electrode in a photoelectrochemcial (PEC) system to simultaneously remove azo-dye and to generate hydrogen in the anodic and cathodic chamber, respectively. The chemical and physical properties of as-synthesized Pd/TNAs were characterized by scanning electron microscopy (SEM), ultraviolet–visible spectroscopy (UV-vis), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). SEM image indicates the diameter and the length of Pd/TNAs were approximately 300 nm and 2.5 μm, respectively. XPS analyses indicate that 1.13% (atomic %) of Pd was loaded onto the surface of TNAs. UV-vis results show that the band gap of TNAs was reduced from 3.2 eV to 2.37 eV after Pd loading. In addition, the electrochemical performances of Pd/TNAs were investigated by photocurrent density test and electrochemical impedance spectroscopy (EIS). The photocurrent (4.0 mA/cm²) of Pd /TNAs was higher than that of the uncoated TNAs (1.4 mA/cm²) at a bias potential of 1 V (vs. Ag/AgCl), indicating that Pd/TNAs-C can effectively separate photogenerated electrons and holes. The mechanism of our PEC system was proposed and discussed in detail in this study.

Keywords: Pd/TNAs, photoelectrochemical, azo-dye degradation, hydrogen generation

Procedia PDF Downloads 392

Authors: H. B. Rekha, Usha N. Murthy, Prashanth, Ashoka

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Dyes are manufactured to have high chemical resistance because they are normally species, very difficult to degrade (reactive dyes). It damages flora and fauna. Furthermore, coloured components are highly hazardous. So removal of dyes becomes a challenge for both textile industry and water treatment facility. Dyeing wastewater is usually treated by conventional methods such as biological oxidation and adsorption but nowadays them becoming in-adequate because of large variability of composition of waste water. In the present investigation, mild steel electrodes of varying surface area were used for treatment of synthetic textile dye. It appears that electro-chemical coagulation could be very effective in removing coloured from wastewater; it could also be used to remove other parameters like chlorides, COD, and solids to some extent. In the present study, coloured removal up to 99% was obtained for surface area of mild steel electrode of 80 cm2 and 96% of surface area of mild steel electrode of 50 cm2. The findings from this study could be used to improve the design of electro-chemical treatment systems and modify existing systems to improve efficiency.

Keywords: electrochemical coagulation, mild steel, colour, environmental engineering

Procedia PDF Downloads 279

Authors: N. Al-Orfi, M. S. El-Shahawi, A. S. Bashammakh

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The electrochemical response of glassy carbon electrode (GCE) for the sensitive and selective determination of dianabol steroid (DS) in phosphate, Britton-Robinson (B-R) and HEPES buffers of pH 2.0 - 11, 2.0 - 11 and 6.2 - 8.0, respectively using cyclic voltammetry (CV) and differential pulse- adsorptive cathodic stripping voltammetry (DP-CSV) at bare GCE was studied. The dependence of the CV response of the developed cathodic peak potential (Ep, c), peak current (ip, c) and the current function (ip, c / υ1/2) on the scan rate (υ) at the bare GCE revealed the occurrence of electrode coupled chemical reaction of EC type mechanism. The selectivity of the proposed method was assessed in the presence of high concentrations of major interfering species e.g. uric acid, ascorbic acid, citric acid, glucose, fructose, sucrose, starch and ions Na+, K+, PO4-3, NO3- and SO42-. The recovery of the method was not significant where t(critical)=2.20 > texp=1.81-1.93 at 95% confidence. The analytical application of the sensor for the quantification of DS in biological fluids as urine was investigated. The results were demonstrated as recovery percentages in the range 95±2.5-97±4.7% with relative standard deviation (RSD) of 0.5-1.5%.

Keywords: dianabol, determination, modified electrode, urine

Procedia PDF Downloads 245