Search results for: electrochemical characterization

Authors: Disha Gupta

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The aim of this research is to conduct X-ray and e-beam characterization techniques on lithium-ion battery materials for the improvement of battery performance. The key characterization techniques employed are the synchrotron X-ray Absorption Spectroscopy (XAS) combined with X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) to obtain a more holistic approach to understanding material properties. This research effort provides additional battery characterization knowledge that promotes the development of new cathodes, anodes, electrolyte and separator materials for batteries, hence, leading to better and more efficient battery performance. Both ex-situ and in-situ synchrotron experiments were performed on LiFePO₄, one of the most common cathode material, from different commercial sources and their structural analysis, were conducted using Athena/Artemis software. This analysis technique was then further extended to study other cathode materials like LiMnxFe(₁₋ₓ)PO₄ and even some sulphate systems like Li₂Mn(SO₄)₂ and Li₂Co0.5Mn₀.₅ (SO₄)₂. XAS data were collected for Fe and P K-edge for LiFePO4, and Fe, Mn and P-K-edge for LiMnxFe(₁₋ₓ)PO₄ to conduct an exhaustive study of the structure. For the sulphate system, Li₂Mn(SO₄)₂, XAS data was collected at both Mn and S K-edge. Finite Difference Method for Near Edge Structure (FDMNES) simulations were also conducted for various iron, manganese and phosphate model compounds and compared with the experimental XANES data to understand mainly the pre-edge structural information of the absorbing atoms. The Fe K-edge XAS results showed a charge compensation occurring on the Fe atom for all the differently synthesized LiFePO₄ materials as well as the LiMnxFe(₁₋ₓ)PO₄ systems. However, the Mn K-edge showed a difference in results as the Mn concentration changed in the materials. For the sulphate-based system Li₂Mn(SO₄)₂, however, no change in the Mn K-edge was observed, even though electrochemical studies showed Mn redox reactions.

Keywords: li-ion batteries, electrochemistry, X-ray absorption spectroscopy, XRD

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Authors: Hang Zhou, Limin Zhu

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This paper investigates the fabrication of microstructures on Si surfaces by using electrochemical anodic oxidation with agarose stamps. The fabricating process is based on a selective anodic oxidation reaction that occurs in the contact area between a stamp and a Si substrate. The stamp which is soaked in electrolyte previously acts as a current flow channel. After forming the oxide patterns as an etching mask, a KOH aqueous is used for the wet etching of Si. A complicated microstructure array of 1 cm2 was fabricated by the method with high accuracy.

Keywords: microstructures, anodic oxidation, silicon, agarose stamps

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Authors: Belal Bakheet, John Beardall, Xiwang Zhang, David McCarthy

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The potential risks associated with toxic cyanobacteria have raised growing environmental and public health concerns leading to an increasing effort into researching ways to bring about their removal from water, together with destruction of their associated cyanotoxins. A variety of toxins are synthesized by cyanobacteria and include hepatotoxins, neurotoxins, and cytotoxins which can cause a range of symptoms in humans from skin irritation to serious liver and nerve damage. Therefore drinking water treatment processes should ensure the consumers’ safety by removing both cyanobacterial cells, and cyanotoxins from the water. Cyanobacterial cells and cyanotoxins presented challenges to the conventional water treatment systems; their accumulation within drinking water treatment plants has been reported leading to plants shut down. Thus, innovative and effective water purification systems to tackle cyanobacterial pollution are required. In recent years there has been increasing attention to the electrochemical oxidation process as a feasible alternative disinfection method which is able to generate in situ a variety of oxidants that would achieve synergistic effects in the water disinfection process and toxin degradation. By utilizing only electric current, the electrochemical process through electrolysis can produce reactive oxygen species such as hydroxyl radicals from the water, or other oxidants such as chlorine from chloride ions present in the water. From extensive physiological and morphological investigation of cyanobacterial cells during electrolysis, our results show that these oxidants have significant impact on cell inactivation, simultaneously with cyanotoxins removal without the need for chemicals addition. Our research aimed to optimize existing electrochemical oxidation systems and develop new systems to treat water containing toxic cyanobacteria and cyanotoxins. The research covers detailed mechanism study on oxidants production and cell inactivation in the treatment under environmental conditions. Overall, our study suggests that the electrochemical treatment process e is an effective method for removal of toxic cyanobacteria and cyanotoxins.

Keywords: toxic cyanobacteria, cyanotoxins, electrochemical process, oxidants

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Authors: Sh. Heidari, A. J. Andrews, A. Oberoi

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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 a roundtrip energy efficiency comparable to lithium ion batteries, while having higher gravimetric and volumetric energy densities. In this paper, a theoretical model is presented of the process of H+ ion (proton) conduction through an acid electrolyte into a highly porous activated carbon electrode where it is neutralised and absorbed on the inner surfaces of pores. A Butler-Volmer type equation relates the rate of adsorption to the potential difference between the activated carbon surface and the electrolyte. This model for the hydrogen storage electrode is then incorporated into a more general computer model based on MATLAB software of the entire electrochemical cell including the oxygen electrode. Hence a theoretical voltage-current curve is generated for given input parameters for a particular activated carbon electrode. It is shown that theoretical VI curves produced by the model can be fitted accurately to experimental data from an actual electrochemical cell with the same characteristics. By obtaining the best-fit values of input parameters, such as the exchange current density and charge transfer coefficient for the hydrogen adsorption reaction, an improved understanding of the adsorption reaction is obtained. This new model will assist in designing improved proton flow batteries for storing solar and wind energy.

Keywords: electrochemical hydrogen storage, proton flow battery, butler-volmer equation, activated carbon

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Authors: Nandini Sharma

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Monitoring the characteristics of a nanostructured material comprises measurements of structural, morphological, mechanical, optical and electronic properties of the synthesized nanopowder and different layers and coatings of nanomaterials coated on transparent conducting oxides (TCOs) substrates like fluorine doped tin oxide (FTO) or Indium doped tin oxide (ITO). This article focuses on structural and optical characterization with emphasis on measurements of the photocatalytic efficiency as a photocatalyst and their interpretation to extract relevant information about various TCOs and materials, their emitter regions, and surface passivation. It also covers a brief description of techniques based on photoluminescence that can portray high resolution pictorial graphs for application as solar energy devices. With the advancement in the scientific techniques, detailed information about the structural, morphological, and optical properties can be investigated, which is further useful for engineering and designing of an efficient device. The common principles involved in the prevalent characterization techniques aid to illustrate the range of options that can be broadened in near future for acurate device characterization and diagnosis.

Keywords: characterization, structural, optical, nanomaterial

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Authors: S. Trafela, X. Xua, K. Zuzek Rozmana

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In this study, we used an accurate and precise method to measure the electrochemically active surface areas (Aecsa) of nickel electrodes. Calculated Aecsa is really important for the evaluation of an electro-catalyst’s activity in electrochemical reaction of different organic compounds. The method involves the electrochemical formation of Ni(OH)₂ and NiOOH in the presence of adsorbed oxalate in alkaline media. The studies were carried out using cyclic voltammetry with polycrystalline nickel as a reference material and electrodeposited nickel nanowires, homogeneous and heterogeneous nickel films. From cyclic voltammograms, the charge (Q) values for the formation of Ni(OH)₂ and NiOOH surface oxides were calculated under various conditions. At sufficiently fast potential scan rates (200 mV s⁻¹), the adsorbed oxalate limits the growth of the surface hydroxides to a monolayer. Although the Ni(OH)₂/NiOOH oxidation peak overlaps with the oxygen evolution reaction, in the reverse scan, the NiOOH/ Ni(OH)₂ reduction peak is well-separated from other electrochemical processes and can be easily integrated. The values of these integrals were used to correlate experimentally measured charge density with an electrochemically active surface layer. The Aecsa of the nickel nanowires, homogeneous and heterogeneous nickel films were calculated to be Aecsa-NiNWs = 4.2066 ± 0.0472 cm², Aecsa-homNi = 1.7175 ± 0.0503 cm² and Aecsa-hetNi = 2.1862 ± 0.0154 cm². These valuable results were expanded and used in electrochemical studies of formaldehyde oxidation. As mentioned nickel nanowires, heterogeneous and homogeneous nickel films were used as simple and efficient sensor for formaldehyde detection. For this purpose, electrodeposited nickel electrodes were modified in 0.1 mol L⁻¹ solution of KOH in order to expect electrochemical activity towards formaldehyde. The investigation of the electrochemical behavior of formaldehyde oxidation in 0.1 mol L⁻¹ NaOH solution at the surface of modified nickel nanowires, homogeneous and heterogeneous nickel films were carried out by means of electrochemical techniques such as cyclic voltammetric and chronoamperometric methods. From investigations of effect of different formaldehyde concentrations (from 0.001 to 0.1 mol L⁻¹) on electrochemical signal - current we provided catalysis mechanism of formaldehyde oxidation, detection limit and sensitivity of nickel electrodes. The results indicated that nickel electrodes participate directly in the electrocatalytic oxidation of formaldehyde. In the overall reaction, formaldehyde in alkaline aqueous solution exists predominantly in form of CH₂(OH)O⁻, which is oxidized to CH₂(O)O⁻. Taking into account the determined (Aecsa) values we have been able to calculate the sensitivities: 7 mA mol L⁻¹ cm⁻² for nickel nanowires, 3.5 mA mol L⁻¹ cm⁻² for heterogeneous nickel film and 2 mA mol L⁻¹ cm⁻² for heterogeneous nickel film. The detection limit was 0.2 mM for nickel nanowires, 0.5 mM for porous Ni film and 0.8 mM for homogeneous Ni film. All of these results make nickel electrodes capable for further applications.

Keywords: electrochemically active surface areas, nickel electrodes, formaldehyde, electrocatalytic oxidation

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Authors: Soukaina Oujana, Peggy Zwolinski

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Fines are heterogeneous residues created during the shredding of non-hazardous waste. They are one of the most challenging issues faced by recyclers, because they are at the present time considered as non-sortable and non-reusable mixtures destined to landfill. However, fines contain a large amount of recoverable materials that could be recycled or reused for the production of solid recovered fuel. This research is conducted in relation to a project named ValoRABES. The aim is to characterize fines and establish a suitable sorting process in order to extract the materials contained in the mixture and define their suitable recovery paths. This paper will highlight the importance of a good sampling and will propose a sampling methodology for fines characterization. First results about the characterization will be also presented.

Keywords: fines, non-hazardous waste, recovery, shredding residues, waste characterization, waste sampling

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Authors: M. H. Belahssen, S. Benramache

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This paper presents corrosion behavior of alloy 42CrMo4 steel nitrided by plasma. Different samples nitrided were tested. The corrosion behavior was evaluated by electrochemical impedance spectroscopy and the tests were carried out in acid chloride solution 1M. The best corrosion protection was observed for nitrided samples. The aim of this work is to compare equivalents circuits corresponding to Nyquist curves simulated and experimental and select who gives best results of impedance parameters with lowest error.

Keywords: pasma nitriding, steel, alloy 42CrMo4, elecrochemistry, corrosion behavior

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Authors: Zawawi Daud

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Agro waste can be defined as waste from agricultural plant. Oil palm leaf and corn stalk can be categorized as ago waste material. At first, the comparison between oil palm leaf and corn stalk by mechanical properties from soda pulping process. After that, focusing on surface characterization by Scanning Electron Microscopy (SEM). Both material have a potential due to mechanical properties (tensile, tear, burst and fold) and surface characterization but corn stalk shows more in strength and compactness due to fiber characterization compared to oil palm leaf. This study promoting the green technology in develop a friendly product and suitable to be used as an alternative pulp in paper making industry.

Keywords: fiber, oil palm leaf, corn stalk, green technology

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Authors: S. B. Mayil Vealan, C. Sekar

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Bisphenol A (BIS A) and 4 Nitrophenol (4N) are the most prevalent environmental endocrine-disrupting chemicals which mimic hormones and have a direct relationship to the development and growth of animal and human reproductive systems. Moreover, intensive exposure to the compound is related to prostate and breast cancer, infertility, obesity, and diabetes. Hence, accurate and reliable determination techniques are crucial for preventing human exposure to these harmful chemicals. Lanthanum Copper Oxide (La₂Cu₂O₅) nanoparticles were synthesized and investigated through various techniques such as scanning electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and electrochemical impedance spectroscopy. Cyclic voltammetry and square wave voltammetry techniques are employed to evaluate the electrochemical behavior of as-synthesized samples toward the electrochemical detection of Bisphenol A and 4-Nitrophenol. Under the optimal conditions, the oxidation current increased linearly with increasing the concentration of BIS A and 4-N in the range of 0.01 to 600 μM with a detection limit of 2.44 nM and 3.8 nM. These are the lowest limits of detection and the widest linear ranges in the literature for this determination. The method was applied to the simultaneous determination of BIS A and 4-N in real samples (food packing materials and river water) with excellent recovery values ranging from 95% to 99%. Better stability, sensitivity, selectivity and reproducibility, fast response, and ease of preparation made the sensor well-suitable for the simultaneous determination of bisphenol and 4 Nitrophenol. To the best of our knowledge, this is the first report in which La₂Cu₂O₅ nano particles were used as efficient electron mediators for the fabrication of endocrine disruptor (BIS A and 4N) chemical sensors.

Keywords: endocrine disruptors, electrochemical sensor, Food contacting materials, lanthanum cuprates, nanomaterials

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Authors: Maria V. Morozova, Zoya A. Mikhaylovskaya, Elena S. Buyanova, Sofia A. Petrova, Ksenia V. Arishina, Robert G. Zaharov

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The present work is devoted to the investigation of two series of doped bismuth molybdates: Bi₂₆-₂ₓMn₂ₓMo₁₀O₆₉-d and Bi₂₆Mo₁₀-₂yMn₂yO₆₉-d. Complex oxides were synthesized by conventional solid state technology and by co-precipitation method. The products were identified by powder diffraction. The powders and ceramic samples were examined by means of densitometry, laser diffraction, and electron microscopic methods. Porosity of the ceramic materials was estimated using the hydrostatic method. The electrical conductivity measurements were carried out using impedance spectroscopy method.

Keywords: bismuth molybdate, columnar structures, impedance spectroscopy, oxygen ionic conductors

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Authors: Jianfang Wang, Xianzhe Chen, Zhuoliang Liu, Cheng-An Tao, Yujiao Li

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Organophosphorus (OPs) pesticide used as insecticides are widely used in agricultural pest control, household and storage deworming. The detection of pesticides needs more simple and efficient methods. One of the best ways is to make electrochemical biosensors. In this paper, an electrochemical enzyme biosensor based on acetylcholine esterase (AChE) was constructed, and its sensing properties and sensing mechanisms were studied. Reduced graphene oxide-polydopamine complexes (RGO-PDA), gold nanoparticles (AuNPs) and silver nanoparticles (AgNPs) were prepared firstly and composited with AChE and chitosan (CS), then fixed on the glassy carbon electrode (GCE) surface to construct the biosensor GCE/RGO-PDA-AuNPs-AgNPs-AChE-CS by one-pot method. The results show that graphene oxide (GO) can be reduced by dopamine (DA) and dispersed well in RGO-PDA complexes. And the composites have a synergistic catalysis effect and can improve the surface resistance of GCE. The biosensor selectively can detect acetylcholine (ACh) and OPs pesticide with good linear range and high sensitivity. The performance of the biosensor is affected by the ratio and adding ways of AChE and the adding of AuNPs and AChE. And the biosensor can achieve a detection limit of 2.4 ng/L for methyl parathion and a wide linear detection range of 0.02 ng/L ~ 80 ng/L, and has excellent stability, good anti-interference ability, and excellent preservation performance, indicating that the sensor has practical value.

Keywords: acetylcholine esterase, electrochemical biosensor, nanoparticles, organophosphates, reduced graphene oxide

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Authors: Charmaine Lamiel, Van Hoa Nguyen, Deivasigamani Ranjith Kumar, Jae-Jin Shim

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The quest for alternative sources of energy storage had led to the exploration on supercapacitors. Hybrid supercapacitors, a combination of carbon-based material and transition metals, had yielded long and improved cycle life as well as high energy and power densities. In this study, microwave irradiation was used for the facile and rapid synthesis of mesoporous RGO@(Co,Mn)3O4 nanosheets as an active electrode material. The advantages of this method include the non-use of reducing agents and acidic medium, and no further post-heat treatment. Additionally, it offers shorter reaction time at low temperature and low power requirement, which allows low fabrication and energy cost. The as-prepared electrode material demonstrated a high capacitance of 953 F•g−1 at 1 A•g−1 in a 6 M KOH electrolyte. Furthermore, the electrode exhibited a high energy density of 76.2 Wh•kg−1 (power density of 720 W•kg−1) and a high power density of 7200 W•kg−1 (energy density of 38 Wh•kg−1). The successful synthesis was considered to be efficient and cost-effective, with very promising electrochemical performance that can be used as an active material in supercapacitors.

Keywords: cobalt manganese oxide, electrochemical, graphene, microwave synthesis, supercapacitor

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Authors: Alvaro Ramírez, Martín Muñoz-Morales, Ester L. Fernández, Javier Llanos

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Carbon blacks are value-added materials typically produced through the incomplete combustion or thermal decomposition of hydrocarbons. This material has been used as catalysts in many different applications, but in last decade it has been explored its potential in green chemistry applications. Among them, the electrochemical production of H2O2 has attracted many interests because of their properties as high oxidant capacity or their industrial interest as bleaching agent. Carbon blacks are commonly used in this application in a catalytic ink that it is drop-casted on supporting electrodes and act as catalysts for the electrochemical production of H₂O₂ through oxygen reduction reaction (ORR). However, according with the different structural and electrochemical behavior of each type, applications might be different. In this line the term ‘carbon black’, has to be considered as a generic name that do not guarantee any properties if any further description was mentioned. In fact, different specific surface area, surface functional groups, porous structure and electro catalysts effect seem very important for electrochemical applications and considerable differences were found during the analysis of four type of carbon blacks. Thus, the aim of this work is to study the evolution of main properties already mentioned to differentiate among some types of carbon blacks and the suitable ones for the ORR to produce H₂O₂ with improved selectivity and efficiency. Results indicate that number and size of porous is one of the key parameters but also the surface functional groups both highly related to the overall process efficiency.

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

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Authors: Yasser M. Abd-elrhman, Mohamed A. Gepreel, Kiochi Nakamura, Ahmed Abd El-Moneim, Sengo Kobayashi, Mervat M. Ibrahim

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Titanium alloys are known as highly bio compatible metallic materials due to their high strength, low elastic modulus, and high corrosion resistance in biological media. Besides other important material features, the corrosion parameters and corrosion products are responsible for limiting the biological and chemical bio compatibility of metallic materials that produce undesirable reactions in implant-adjacent and/or more distant tissues. Electrochemical corrosion behaviors of novel beta titanium alloys, Ti-4.7Mo-4.5Fe, Ti-3Mo-0.5Fe, and Ti-2Mo-0.5Fe were characterized in naturally aerated Ringer’s solution at room temperature compared with common used biomedical titanium alloy, Ti-6Al-4V. The corrosion resistance of titanium alloys were investigated through open circuit potential (OCP), potentiodynamic polarization measurements and optical microscope (OM). A high corrosion resistance was obtained for all alloys due to the stable passive film formed on their surfaces. The new present alloys are promising metallic biomaterials for the future, owing to their very low elastic modulus and good corrosion resistance capabilities.

Keywords: titanium alloys, corrosion resistance, Ringer’s solution, electrochemical corrosion

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Authors: Shah Abbas

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Rheumatoid arthritis is a systemic, inflammatory autoimmune disease, affecting an overall 1% of the global population. Despite being tremendous efforts by scientists, early diagnosis of RA still has not been achieved. In the current study, a Graphene oxide (GO) based electrochemical sensor has been developed for early diagnosis of RA through Cyclic voltammetry. Chitosan (CHI), a CPnatural polymer has also been incorporated along with GO in order to enhance the biocompatibility and functionalization potential of the biosensor. CCPs are known antigens for Anti Citrullinated Peptide Antibodies (ACPAs) which can be detected in serum even 14 years before the appearance of symptoms, thus they are believed to be an ideal target for the early diagnosis of RA. This study has yielded some promising results regarding the binding and detection of ACPAs through changes in the electrochemical properties of biosensing material. The cyclic voltammogram of this biosensor reflects the binding of ACPAs to the biosensor surface, due to its shifts observed in the current flow (cathodic current) as compared to the when no ACPAs bind as it is absent in RA negative patients.

Keywords: rheumatoid arthritis, peptide sensor, graphene oxide, anti citrullinated peptide antibodies, cyclic voltammetry

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Authors: Sofia G. Meirinho, Luis G. Dias, António M. Peres, Lígia R. Rodrigues

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The emerging development of electrochemical aptasen sors has enabled the easy and fast detection of protein biomarkers in standard and real samples. Biomarkers are produced by body organs or tumours and provide a measure of antigens on cell surfaces. When detected in high amounts in blood, they can be suggestive of tumour activity. These biomarkers are more often used to evaluate treatment effects or to assess the potential for metastatic disease in patients with established disease. Osteopontin (OPN) is a protein found in all body fluids and constitutes a possible biomarker because its overexpression has been related with breast cancer evolution and metastasis. Currently, biomarkers are commonly used for the development of diagnostic methods, allowing the detection of the disease in its initial stages. A previously described RNA aptamer was used in the current work to develop a simple and sensitive electrochemical aptasensor with high affinity for human OPN. The RNA aptamer was biotinylated and immobilized on a gold electrode by avidin-biotin interaction. The electrochemical signal generated from the aptamer–target molecule interaction was monitored electrochemically using cyclic voltammetry in the presence of [Fe (CN) 6]−3/− as a redox probe. The signal observed showed a current decrease due to the binding of OPN. The preliminary results showed that this aptasensor enables the detection of OPN in standard solutions, showing good selectivity towards the target in the presence of others interfering proteins such as bovine OPN and bovine serum albumin. The results gathered in the current work suggest that the proposed electrochemical aptasensor is a simple and sensitive detection tool for human OPN and so, may have future applications in cancer disease monitoring.

Keywords: osteopontin, aptamer, aptasensor, screen-printed electrode, cyclic voltammetry

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Authors: Jigar Shaileshumar Halpati, Aravind Kumar Chandiran

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Vacancy ordered double perovskites (VOPs) have been significantly attracting researchers due to their chemical structure diversity and interesting optoelectronic properties. Some VOPs have been recently reported to be suitable photoelectrodes for photoelectrochemical water-splitting reactions due to their high stability and panchromatic absorption. In this work, we systematically synthesized mixed tetravalent VOPs based on Cs₂RuₘPt₁-ₘX₆ (X = Cl-, Br-) and reported their structural, optical, electrochemical and photoelectrochemical properties. The structural characterization confirms that the mixed tetravalent site intermediates formed their own phases. The parent materials, as well as their intermediates, were found to be stable in ambient conditions for over 1 year and also showed incredible stability in harsh pH media ranging from pH 1 to pH 11. Moreover, these materials showed panchromatic absorption with onset up to 1000 nm depending upon the mixture stoichiometry. The extraordinary stability and excellent absorption properties make them suitable materials for photoelectrochemical water-splitting applications. PEC studies of these series of materials showed a high water oxidation photocurrent of 0.56 mA cm-² for Cs₂Ru₀.₅Pt₀.₅Cl₆. Fundamental investigation from photoelectrochemical reactions revealed that the intrinsic ruthenium-based VOP showed enhanced hole transfer to the electrolyte, while the intrinsic platinum-based VOP showed higher photovoltage. The mix of these end members at the tetravalent site showed a synergic effect of reduced charge transfer resistance from the material to the electrolyte and increased photovoltage, which led to increased PEC performance of the intermediate materials.

Keywords: solar water splitting, photo electrochemistry, photo absorbers, material characterization, device characterization, green hydrogen

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Authors: Franky Michael Hamonangan Siagian, Affan Maulana, Himawan Tri Bayu Murti Petrus, Widi Astuti

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In this study, the feasibility of the direct electrowinning method was used to produce zero-valent iron from red mud. The bauxite residue sample came from the Tayan mine, Indonesia, which contains high hematite (Fe₂O₃). Before electrolysis, the samples were characterized by various analytical techniques (ICP-AES, SEM, XRD) to determine their chemical composition and mineralogy. The direct electrowinning method of red mud suspended in NaOH was introduced at low temperatures ranging from 30 - 110 °C. Variations of current density, red mud: NaOH ratio and temperature were carried out to determine the optimum operation of the direct electrowinning process. Cathode deposits and residues in electrochemical cells were analyzed using XRD, XRF, and SEM to determine the chemical composition and current recovery. The low-temperature electrolysis current efficiency on Redmud can reach 20% recovery at a current density of 920,945 A/m². The moderate performance of the process was investigated with red mud, which was attributed to the troublesome adsorption of red mud particles on the cathode, making the reduction far less efficient than that with hematite.

Keywords: red mud, electrochemical reduction, Iron production, hematite

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Authors: Zohreh Derikvand

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One new 2D metal-organic coordination polymer of Ni(II) namely [Ni2(ndc)2(DMSO)4(H2O)]n, where ndc = naphthalene-1,4-dicarboxylic acid and DMSO= dimethyl sulfoxide has been synthesized and characterized by elemental analysis, spectral (IR, UV-Vis), thermal (TG/DTG) analysis and single crystal X-ray diffraction. Compound 1 possesses a 2D layer structure constructed from dinuclear nickel(II) building blocks in which two crystallographically independent Ni2+ ions are bridged by ndc2– ligands and water molecule. The ndc2– ligands adopt μ3 bridging modes, linking the metal centers into a two-dimensional coordination framework. The two independent NiII cations are surrounded by dimethyl sulfoxide and naphthalene-1,4-dicarboxylate molecules in distorted octahedron geometry. In the crystal structures of 1 there are non-classical hydrogen bonding arrangements and C-H–π stacking interactions. Electrochemical behavior of [Ni2(ndc)2(DMSO)4(H2O)]n, (Ni-NDA) on the surface of carbon nanotube (CNTs) glassy carbon electrode (GCE) was described. The surface structure and composition of the sensor were characterized by scanning electron microscopy (SEM). Oxidation of fructose on the surface of modified electrode was investigated with cyclic voltammetry and electrochemical impedance spectroscopy (EIS) and the results showed that the Ni-NDA/CNTs film displays excellent electrochemical catalytic activities towards fructose oxidation.

Keywords: naphthalene-1, 4-dicarboxylic acid, crystal structure, coordination polymer, electrocatalysis, impedance spectroscopy

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Authors: Cyril O. Ehi-Eromosele, Ajayi Kayode

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The Li-rich layered metal oxides (LLO) are the most promising candidates for promising electrodes of high energy Li-ion battery (LIB). In literature, these electrode system has either been designed as a hetero-structure of the primary components (composite) or as a core-shell structure with improved electrochemistry reported for both configurations when compared with its primary components. With the on-going efforts to improve on the electrochemical performance of the LIB, it is important to investigate comparatively the structural and electrochemical characteristics of the core-shell like and ‘composite’ forms of these materials with the same compositions and synthesis conditions which could influence future engineering of these materials. Therefore, this study concerns the structural and electrochemical properties of the ‘composite’ and core-shell like LLO cathode materials with the same nominal composition of 0.5Li₂MnO₃-0.5LiNi₀.₅Mn₀.₃Co₀.₂O₂ (LiNi₀.₅Mn₀.₃Co₀.₂O₂ as core and Li₂MnO₃ as the shell). The results show that the core-shell sample (–CS) gave better electrochemical performance than the ‘composite’ sample (–C). Both samples gave the same initial charge capacity of ~300 mAh/g when cycled at 10 mA/g and comparable charge capacity (246 mAh/g for the –CS sample and 240 mAh/g for the –C sample) when cycled at 200 mA/g. However, the –CS sample gave a higher initial discharge capacity at both current densities. The discharge capacity of the –CS sample was 232 mAh/g and 164 mAh/g while the –C sample is 208 mAh/g and 143 mAh/g at the current densities of 10 mA/g and 200 mA/g, respectively. Electrochemical impedance spectroscopy (EIS) results show that the –CS sample generally exhibited a smaller resistance than the –C sample both for the uncycled and after 50th cycle. Detailed structural analysis is on-going, but preliminary results show that the –CS sample had bigger unit cell volume and a higher degree of cation mixing. The thermal stability of the –CS sample was higher than the –C sample. XPS investigation also showed that the pristine –C sample gave a more reactive surface (showing formation of carbonate species to a greater degree) which could result in the greater resistance seen in the EIS result. To reinforce the results obtained for the 0.5Li₂MnO₃-0.5LiNi₀.₅Mn₀.₃Co₀.₃O₂ composition, the same investigations were extended to another ‘composite’ and core-shell like LLO cathode materials also with the same nominal composition of 0.5Li₂MnO₃-0.5LiNi₀.₃Mn₀.₃Co₀.₃O₂. In this case, the aim was to determine the electrochemical performance of the material using a low Ni content (LiNi₀.₃Mn₀.₃Co₀.₃O₂) as the core to clarify the contributions of the core-shell configuration to the electrochemical performance of these materials. Ni-rich layered oxides show active catalytic surface leading to electrolyte oxidation resulting in poor thermal stability and cycle life. Here, the core-shell sample also gave better electrochemical performance than the ‘composite’ sample with 0.5Li₂MnO₃-0.5LiNi₀.₃Mn₀.₃Co₀.₃O₂ composition. Furthermore, superior electrochemical performance was also recorded for the core-shell like spinel modified LLO (0.5Li₂MnO₃-0.45LiNi₀.₅Mn₀.₃Co₀.₂O₂-0.05LiNi₀.₅Mn₁.₅O₄) when compared to the composite system. These results show that the core-shell configuration can generally be used to improve the structural and electrochemical properties of the LLO and spinel modified LLO materials.

Keywords: lithium-ion battery, lithium rich oxide cathode, core-shell structure, composite structure

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Authors: Mohadeseh Seyednezhad, Armin Rajabi, Andanastui Muchtar, Mahendra Rao Somalu

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This work investigates the electrical properties of NiO-SDC/SDC anode sintered at about 1200 ○C for 1h through a relatively new approach, namely the microwave method. Nano powders Sm0.2Ce0.8O1.9 (SDC) and NiO were mixed by using a high-energy ball-mill and subsequent co-pressed at three different compaction pressures 200, 300 and 400 MPa. The novelty of this study consists in the effect of compaction pressure on the electrochemical performance of Ni-SDC/SDC anode, with no binder used between layers. The electrical behavior of the prepared anode has been studied by electrochemical impedance spectra (EIS) in controlled atmospheres, operating at high temperatures (600-800 °C).

Keywords: sintering, fuel cell, electrical conductivity, nanostructures, impedance spectroscopy, ceramics

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Authors: Franky Michael Hamonangan Siagian, Affan Maulana, Himawan Tri Bayu Murti Petrus, Panut Mulyono, Widi Astuti

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In this study, the feasibility of the direct electrowinning method was used to produce zero-valent iron from red mud. The bauxite residue sample came from the Tayan mine, Indonesia, which contains high hematite (Fe₂O₃). Before electrolysis, the samples were characterized by various analytical techniques (ICP-AES, SEM, XRD) to determine their chemical composition and mineralogy. The direct electrowinning method of red mud suspended in NaOH was introduced at low temperatures ranging from 30 - 110 °C. Variations of current density, red mud: NaOH ratio and temperature were carried out to determine the optimum operation of the direct electrowinning process. Cathode deposits and residues in electrochemical cells were analyzed using XRD, XRF, and SEM to determine the chemical composition and current recovery. The low-temperature electrolysis current efficiency on Redmud can reach 20% recovery at a current density of 920,945 A/m². The moderate performance of the process was investigated with red mud, which was attributed to the troublesome adsorption of red mud particles on the cathode, making the reduction far less efficient than that with hematite.

Keywords: alumina, red mud, electrochemical reduction, iron production

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Authors: Kun-Ting Song, Christian Schott, Peter Schneider, Sebastian Watzele, Regina Kluge, Elena Gubanova, Aliaksandr S. Bandarenka

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The combination of electrochemical impedance spectroscopy (EIS) and the hydrodynamic technique like rotation disc electrode (RDE) provides a critical method for quantitively investigating mechanisms of hydrogen evolution reaction (HER) in acidic and alkaline media. Pt5Gd represented higher HER activities than polycrystalline Pt (Pt(pc)) by means of the surface strain effects. The model of the equivalent electric circuit to fit the impedance data under the RDE configurations is developed. To investigate the relative reaction contribution, the ratio of the charge transfer reactions of the Volmer-Heyrovsky and Volmer-Tafel pathways on Pt and Pt5Gd electrodes is determined. The ratio remains comparably similar in acidic media, but it changes in alkaline media with Volmer–Heyrovsky pathway dominating. This combined approach of EIS and RDE can help to study the electrolyte effects and other essential reactions for electrocatalysis in future work.

Keywords: hydrogen evolution reaction, electrochemical impedance spectroscopy, hydrodynamic methods, electrocatalysis, electrochemical interface

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Authors: Boriana Karamanova, Svetlana Veleva, Luybomir Soserov, Ana Arenillas, Francesco Lufrano, Antonia Stoyanova

Abstract:

Supercapacitors have received a lot of research attention and are promising energy storage devices due to their high power and long cycle life. In order to developed an advanced device with significant capacity for storing charge and cheap carbon materials, efforts must focus not only on improving synthesis by controlling the morphology and pore size but also on improving electrode-electrolyte compatibility of the resulting systems. The present study examines the relationship between the surface chemistry of two activated carbon xerogels, the electrolyte type, and the electrochemical properties of supercapacitors. Activated carbon xerogels were prepared by varying the initial pH of the resorcinol-formaldehyde aqueous solution. The materials produced are physicochemical characterized by DTA/TGA, porous characterization, and SEM analysis. The carbon xerogel based electrodes were prepared by spreading over glass plate a slurry containing the carbon gel, graphite, and poly vinylidene difluoride (PVDF) binder. The layer formed was dried consecutively at different temperatures and then detached by water. After, the layer was dried again to improve its mechanical stability. The developed electrode materials and the Aquivion® E87-05S membrane (Solvay Specialty Polymers), socked in Na2SO4 as a polymer electrolyte, were used to assembly the solid-state supercapacitor. Symmetric supercapacitor cells composed by same electrodes and 1 M KOH electrolytes are also assembled and tested for comparison. The supercapacitor performances are verified by different electrochemical methods - cyclic voltammetry, galvanostatic charge/discharge measurements, electrochemical impedance spectroscopy, and long-term durability tests in neutral and alkaline electrolytes. Specific capacitances, energy, and power density, energy efficiencies, and durability were compared into studied supercapacitors. Ex-situ physicochemical analyses on the synthesized materials have also been performed, which provide information about chemical and structural changes in the electrode morphology during charge / discharge durability tests. They are discussed on the basis of electrode-electrolyte interaction. The obtained correlations could be of significance in order to design sustainable solid-state supercapacitors with high power and energy density. Acknowledgement: This research is funded by the Ministry of Education and Science of Bulgaria under the National Program "European Scientific Networks" (Agreement D01-286 / 07.10.2020, D01-78/30.03.2021). Authors gratefully acknowledge.

Keywords: carbon xerogel, electrochemical tests, neutral and alkaline electrolytes, supercapacitors

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Authors: V. Pérez-Herranz, M. Pinel, E. M. Ortega, M. García-Gabaldón

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In the present work, Electrochemical Impedance Spectrocopy (EIS) is applied to study the transport of different metal cations through a cation-exchange membrane. This technique enables the identification of the ionic-transport characteristics and to distinguish between different transport mechanisms occurring at different current density ranges. The impedance spectra are dependent on the applied dc current density, on the type of cation and on the concentration. When the applied dc current density increases, the diameter of the impedance spectra loops increases because all the components of membrane system resistance increase. The diameter of the impedance plots decreases in the order of Na(I), Ni(II) and Cr(III) due to the increased interactions between the negatively charged sulfonic groups of the membrane and the cations with greater charge. Nyquist plots are shifted towards lower values of the real impedance, and its diameter decreases with the increase of concentration due to the decrease of the solution resistance.

Keywords: ion-exchange membranes, Electrochemical Impedance Spectrocopy, multivalent metal cations, membrane system

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Authors: Ahmed A. Farag, M. A. Hgazy

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The influence of three Schiff bases (SB-I, SB-II, and SB-III) on the corrosion of carbon steel in 0.5 M H2SO4 solution was studied by potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) techniques. The inhibition efficiency increases with the concentration of the Schiff bases and follow the trend: SB-III > SB-II > SB-I. Tafel polarization measurements revealed that the three tested inhibitors function as anodic inhibitors. The thermodynamic parameters Kads and ΔGºads are calculated and discussed. The Langmuir isotherm equation was found to provide an accurate description of the adsorption behaviour of the investigated Schiff bases. Depending on the results, the inhibitive mechanism was proposed.

Keywords: Schiff bases, corrosion inhibitors, EIS, adsorption

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Authors: Ipek Gunay, Efe B. Orman, Metin Ozer, Bekir Salih, Ali R. Ozkaya

Abstract:

Phthalocyanines with macrocyclic ring containing at least three heteroatoms have nine or more membered structures. Metal-free phthalocyanines react with metal salts to obtain chelate complexes. This is one of the most important features of metal-free phthalocyanine as ligand structure. Although phthalocyanines have very similar properties with porphyrins, they have some advantages such as lower cost, easy to prepare, and chemical and thermal stability. It’s known that Pc compounds have shown one-electron metal-and/or ligand-based reversible or quasi-reversible reduction and oxidation processes. The redox properties of phthalocyanines are critically related to the desirable properties of these compounds in their technological applications. Thus, Pc complexes have also been receiving increasing interest in the area of fuel cells due to their high electrocatalytic activity in dioxygen reduction and fuel cell applications. In this study, novel phthalocyanine complexes coordinated with Fe(II) and Co (II) to be used as catalyst were synthesized. Aiming this goal, a new nitrile ligand was synthesized starting from 4-hydroxy-3,5-dimethoxy benzyl alcohol and 4-nitrophthalonitrile in the presence of K2CO3 as catalyst. After the isolation of the new type of nitrile and metal complexes, the characterization of mentioned compounds was achieved by IR, H-NMR and UV-vis methods. In addition, the electrochemical behaviour of Pc complexes was identified by cyclic voltammetry, square wave voltammetry and in situ spectroelectrochemical measurements. Furthermore, the catalytic performances of Pc complexes for oxygen reduction were tested by dynamic voltammetry measurements, carried out by the combined system of rotating ring-disk electrode and potentiostat, in a medium similar to fuel-cell working conditions.

Keywords: phthalocyanine, electrocatalysis, electrochemistry, in-situ spectroelectrochemistry

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Authors: M. Dekmouche, M. Hadjada, Z. Rahmani, M. Saidi

Abstract:

The effect of iodide ions on the corrosion inhibition of mild steel in 20% sulfuric acid in the presence of 3-méthylthio-5-p-méthoxyphényl-1,2-dithiolylium against anion (I-) A1 synthesized in our laboratory,was studied by different electrochemical techniques such as electrochemical impedance spectroscopy, potentiodynamic polarization. The obtained results showed that A1 effectively reduces the corrosion rate of steel. The adsorption of 3-méthylthio-5-p-méthoxyphényl-1,2-dithiolylium against anion (I-) followed Langmuir and temkin adsorption isotherm.

Keywords: steel XC52, corrosion, inhibition, 3-méthylthio-5-p-méthoxyphényl-1, 2-dithiolylium against anion (I-) , sulfuric acid

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Authors: Sudkate Chaiyo, Weena Siangproh, Orawon Chailapakul, Kurt Kalcher

Abstract:

In the present work, a simple and sensitive non-enzymatic electrochemical detection of glucose in disposable paper-based sensor was developed at ionic liquid/graphene/cobalt phthalocyanine composite (IL/G/CoPc) modified electrode. The morphology of the fabricated composite was characterized and confirmed by scanning electron microscopy and UV-Vis spectroscopy. The UV-Vis spectroscopy results confirmed that the G/CoPc composite formed via the strong π–π interaction between CoPc and G. Amperometric i-t technique was used for the determination of glucose. The response of glucose was linear over the concentration ranging from 10 µM to 1.5 mM. The response time of the sensor was found as 30 s with a limit of detection of 0.64 µM (S/N=3). The fabricated sensor also exhibited its good selectivity in the presence of common interfering species. In addition, the fabricated sensor exhibited its special advantages such as low working potential, good sensitivity along with good repeatability and reproducibility for the determination of glucose.

Keywords: glucose, paper-based sensor, ionic liquid/graphene/cobalt phthalocyanine composite, electrochemical detection

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