Search results for: electrochemical techniques

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: Ece Kök Yetimoğlu, Soner Çubuk, Neşe Taşci, M. Vezir Kahraman

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Lead(II) is one of the most toxic environmental pollutants in the world, due to its high toxicity and non-biodegradability. Lead exposure causes severe risks to human health such as central brain damages, convulsions, kidney damages, and even death. To determine lead(II) in environmental or biological samples, scientists use atomic absorption spectrometry (AAS), inductively coupled plasma mass spectrometry (ICPMS), fluorescence spectrometry and electrochemical techniques. Among these systems the fluorescence spectrometry and fluorescent chemical sensors have attracted considerable attention because of their good selectivity and high sensitivity. The fluorescent polymers usually contain covalently bonded fluorophores. In this study imidazole based UV cured polymeric film was prepared and designed to act as a fluorescence chemo sensor for lead (II) analysis. The optimum conditions such as influence of pH value and time on the fluorescence intensity of the sensor have also been investigated. The sensor was highly sensitive with a detection limit as low as 1.87 × 10−8 mol L-1 and it was successful in the determination of Pb(II) in water samples.

Keywords: fluorescence, lead(II), photopolymerization, polymeric sensor

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Authors: Leila Samiee, Amir Yadegari, Saeedeh Tasharrofi

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In the work presented here, nitrogen-doped graphene materials were synthesized and used as metal-free electrocatalysts for oxygen reduction reaction (ORR) under alkaline conditions. Paraphenylenediamine was used as N precursor. The N-doped graphene was synthesized under hydrothermal treatment at 200°C. All the materials have been characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM) and X-ray photo-electron spectroscopy (XPS). Moreover, for electrochemical evaluation of samples, Rotating Disk electrode (RDE) and Cyclic Voltammetry techniques (CV) were employed. The resulting material exhibits an outstanding catalytic activity for the oxygen reduction reaction (ORR) as well as excellent resistance towards methanol crossover effects, indicating their promising potential as ORR electrocatalysts for alkaline fuel cells.

Keywords: alkaline fuel cell, graphene, metal-free catalyst, paraphenylen diamine

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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: 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

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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

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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

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Authors: Dina Ibrahim Abouelamaiem, Ana Jorge Sobrido, Magdalena Titirici, Paul R. Shearing, Daniel J. L. Brett

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Global warming and scarcity of fossil fuels have had a radical impact on the world economy and ecosystem. The urgent need for alternative energy sources has hence elicited an extensive research for exploiting efficient and sustainable means of energy conversion and storage. Among various electrochemical systems, supercapacitors attracted significant attention in the last decade due to their high power supply, long cycle life compared to batteries and simple mechanism. Recently, the performance of these devices has drastically improved, as tuning of nanomaterials provided efficient charge and storage mechanisms. Carbon materials, in various forms, are believed to pioneer the next generation of supercapacitors due to their attractive properties that include high electronic conductivities, high surface areas and easy processing and functionalization. Cellulose has eco-friendly attributes that are feasible to replace man-made fibers. The carbonization of cellulose yields carbons, including activated carbon and graphite fibers. Activated carbons successively are the most exploited candidates for supercapacitor electrode materials that can be complemented with pseudocapacitive materials to achieve high energy and power densities. In this work, the optimum functionalization conditions of cellulose have been investigated for supercapacitor electrode materials. The precursor was treated with potassium hydroxide (KOH) at different KOH/cellulose ratios prior to the carbonization process in an inert nitrogen atmosphere at 850 °C. The chalky products were washed, dried and characterized with different techniques including transmission electron microscopy (TEM), x-ray tomography and nitrogen adsorption-desorption isotherms. The morphological characteristics and their effect on the electrochemical performances were investigated in two and three-electrode systems. The KOH/cellulose ratios of 0.5:1 and 1:1 exhibited the highest performances with their unique hierarchal porous network structure, high surface areas and low cell resistances. Both samples acquired the best results in three-electrode systems and coin cells with specific gravimetric capacitances as high as 187 F g-1 and 20 F g-1 at a current density of 1 A g-1 and retention rates of 72% and 70%, respectively. This is attributed to the morphology of the samples that constituted of a well-balanced micro-, meso- and macro-porosity network structure. This study reveals that the electrochemical performance doesn’t solely depend on high surface areas but also an optimum pore size distribution, specifically at low current densities. The micro- and meso-pore contribution to the final pore structure was found to dominate at low KOH loadings, reaching ‘equilibrium’ with macropores at the optimum KOH loading, after which macropores dictate the porous network. The wide range of pore sizes is detrimental for the mobility and penetration of electrolyte ions in the porous structures. These findings highlight the influence of various morphological factors on the double-layer capacitances and high performance rates. In addition, they open a platform for the investigation of the optimized conditions for double-layer capacitance that can be coupled with pseudocapacitive materials to yield higher energy densities and capacities.

Keywords: carbon, electrochemical performance, electrodes, KOH/cellulose optimized ratio, morphology, supercapacitor

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Authors: Gökçe Erdemir, İlhan Yaylım, Serap Erdem-Kuruca, Musa Mutlu Can

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It has been determined that the main reason for the death of cancer disease is caused by metastases rather than the primary tumor. The cells that leave the primary tumor and enter the circulation and cause metastasis in the secondary organs are called "circulating tumor cells" (CTCs). The presence and number of circulating tumor cells has been associated with poor prognosis in many major types of cancer, including breast, prostate, and colorectal cancer. It is thought that knowledge of circulating tumor cells, which are seen as the main cause of cancer-related deaths due to metastasis, plays a key role in the diagnosis and treatment of cancer. The fact that tissue biopsies used in cancer diagnosis and follow-up are an invasive method and are insufficient in understanding the risk of metastasis and the progression of the disease have led to new searches. Liquid biopsy tests performed with a small amount of blood sample taken from the patient for the detection of CTCs are easy and reliable, as well as allowing more than one sample to be taken over time to follow the prognosis. However, since these cells are found in very small amounts in the blood, it is very difficult to capture them and specially designed analytical techniques and devices are required. Methods based on the biological and physical properties of the cells are used to capture these cells in the blood. Early diagnosis is very important in following the prognosis of tumors of epithelial origin such as breast, lung, colon and prostate. Molecules such as EpCAM, vimentin, and cytokeratins are expressed on the surface of cells that pass into the circulation from very few primary tumors and reach secondary organs from the circulation, and are used in the diagnosis of cancer in the early stage. For example, increased EpCAM expression in breast and prostate cancer has been associated with prognosis. These molecules can be determined in some blood or body fluids to be taken from patients. However, more sensitive methods are required to be able to determine when they are at a low level according to the course of the disease. The aim is to detect these molecules found in very few cancer cells with the help of sensitive, fast-sensing biosensors, first in breast cancer cells reproduced in vitro and then in blood samples taken from breast cancer patients. In this way, cancer cells can be diagnosed early and easily and effectively treated.

Keywords: electrochemical biosensors, breast cancer, circulating tumor cells, EpCAM, Vimentin, Cytokeratins

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Authors: Umesh Kumar Soni, Suresh Kumar Soni, S. R. Awasthi

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Worldwide biggest difficulties are climate change, future availability of fossil fuels, and economical feasibility of renewable energy. They force us to use to a greater extent renewable energy and develop suitable hybrid renewable systems. Building heating/cooling consumes significant amount of energy. It can be conserved by use of proper heating/cooling techniques. This paper reviews and critically analyzes various active, passive and hybrid heating/cooling techniques used in green buildings.

Keywords: natural ventilation, energy conservation, hybrid ventilation techniques, climate change

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Authors: Gabriel Wosiak, Jeyse da Silva, Sthefany S. Sena, Renato N. de Andrade, Ernesto Pereira

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The bubble formation during hydrogen production by electrolysis and several electrochemical processes is an inherent phenomenon and can impact the energy consumption of the processes. In this work, it was reported both experimental and computational results describe the effect of bubble displacement, which, under the cases investigated, leads to the formation of a convective flow in the solution. The process is self-sustained, and a solution vortex is formed, which modifies the bubble growth and covering at the electrode surface. Using the experimental data, we have built a model to simulate it, which, with high accuracy, describes the phenomena. Then, it simulated many different experimental conditions and evaluated the effects of the boundary conditions on the bubble surface covering the surface. We have observed a position-dependent bubble covering the surface, which has an effect on the water-splitting efficiency. It was shown that the bubble covering is not uniform at the electrode surface, and using statistical analysis; it was possible to evaluate the influence of the gas type (H2 and O2), current density, and the bubble size (and cross-effects) on the covering fraction and the asymmetric behavior over the electrode surface.

Keywords: water splitting, bubble, electrolysis, hydrogen production

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Authors: T. Abohalkuma, J. Telegdi

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

Keywords: nanolayers, corrosion, phosphonic acids, coatings

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Authors: Rinlee Butch M. Cervera, Princess Stephanie P. Llanos

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Lithium iron phosphate (LiFePO₄) is a potential cathode material for lithium-ion batteries due to its promising characteristics. In this study, pure LiFePO₄ (LFP) and carbon-coated nanograined LiFePO₄ (LFP-C) is synthesized and characterized for its microstructural properties. X-ray diffraction patterns of the synthesized samples can be indexed to an orthorhombic LFP structure with about 63 nm crystallite size as calculated by using Scherrer’s equation. Agglomerated particles that range from 200 nm to 300 nm are observed from scanning electron microscopy images. Transmission electron microscopy images confirm the crystalline structure of LFP and coating of amorphous carbon layer. Elemental mapping using energy dispersive spectroscopy analysis revealed the homogeneous dispersion of the compositional elements. In addition, galvanostatic charge and discharge measurements were investigated for the cathode performance of the synthesized LFP and LFP-C samples. The results showed that the carbon-coated sample demonstrated the highest capacity of about 140 mAhg^-1 as compared to non-coated and micrograined sized commercial LFP.

Keywords: ceramics, energy storage, electrochemical measurements, transmission electron microscope

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Authors: A. Saurabh Singh, B. Raghvendra, C. Prabhakar Singh

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Solid Oxide Fuel Cells (SOFCs) are one of the most attractive electrochemical energy conversion systems, as these devices present a clean energy production, thus promising high efficiencies and low environmental impact. The electrodes are the main components that decisively control the performance of a SOFC. Conventional, anode materials (like Ni-YSZ) are operates at very high temperature. Therefore, cost-effective materials which operate at relatively lower temperatures are still required. In present study, we have synthesized La doped Strontium Titanate via solid state reaction route. The structural, microstructural and density of the pellet have been investigated employing XRD, SEM and Archimedes Principle, respectively. The electrical conductivity of the systems has been determined by impedance spectroscopy techniques. The electrical conductivity of the Lanthanum Strontium Titanate (LST) has been found to be higher than the composite Ni-YSZ system at 700 °C.

Keywords: IT-SOFC, LST, Lanthanum Strontium Titanate, electrical conductivity

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Authors: Vijay Pal Singh, Yogesh Chandra Kotiyal

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Structures are a combination of various load carrying members which transfer the loads to the foundation from the superstructure safely. At the design stage, the loading of the structure is defined and appropriate material choices are made based upon their properties, mainly related to strength. The strength of materials kept on reducing with time because of many factors like environmental exposure and deformation caused by unpredictable external loads. Hence, to predict the strength of materials used in structures, various techniques are used. Among these techniques, Non-Destructive Techniques (NDT) are the one that can be used to predict the strength without damaging the structure. In the present study, the compressive strength of concrete has been predicted using Artificial Neural Network (ANN). The predicted strength was compared with the experimentally obtained actual compressive strength of concrete and equations were developed for different models. A good co-relation has been obtained between the predicted strength by these models and experimental values. Further, the co-relation has been developed using two NDT techniques for prediction of strength by regression analysis. It was found that the percentage error has been reduced between the predicted strength by using combined techniques in place of single techniques.

Keywords: rebound, ultra-sonic pulse, penetration, ANN, NDT, regression

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Authors: Sarmiza Stanca, Wolfgang Fritzsche, Christoph Krafft, Jürgen Popp

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Independent of the cell type a thin layer of a few nanometers thickness surrounds the cell interior as the cellular membrane. The transport of ions and molecules through the membrane is achieved in a very precise way by pores. Understanding the process of opening and closing the pores due to an electrochemical gradient across the membrane requires knowledge of the pore constitutive proteins. Recent reports prove the access to the molecular level of the cellular membrane by atomic force microscopy (AFM). This technique also permits an electrochemical study in the immediate vicinity of the tip. Specific molecules can be electrochemically localized in the natural cellular membrane. Our work aims to recognize the protein domains of the pores using an AFM probe as a miniaturized amperometric sensor, and to follow the protein behavior while changing the applied potential. The intensity of the current produced between the surface and the AFM probe is amplified and detected simultaneously with the surface imaging. The AFM probe plays the role of the working electrode and the substrate, a conductive glass on which the cells are grown, represent the counter electrode. For a better control of the electric potential on the probe, a third electrode Ag/AgCl wire is mounted in the circuit as a reference electrode. The working potential is applied between the electrodes with a programmable source and the current intensity in the circuit is recorded with a multimeter. The applied potential considers the overpotential at the electrode surface and the potential drop due to the current flow through the system. The reported method permits a high resolved electrochemical study of the protein domains on the living cell membrane. The amperometric map identifies areas of different current intensities on the pore depending on the applied potential. The reproducibility of this method is limited by the tip shape, the uncontrollable capacitance, which occurs at the apex and a potential local charge separation.

Keywords: AFM, sensor, membrane, pores, proteins

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Authors: S. Delpeux-Ouldriane, M. Gineys, S. Masson, N. Cohaut, L. Reinert, L. Duclaux, F. Béguin

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Nowadays, a wide variety of organic contaminants are present at trace concentrations in wastewater effluents. In order to face these pollution problems, the implementation of the REACH European regulation has defined lists of targeted pollutants to be eliminated selectively in water. It therefore implies the development of innovative and more efficient remediation techniques. In this sense, adsorption processes can be successfully used to achieve the removal of organic compounds in waste water treatment processes, especially at low pollutant concentration. Especially, activated carbons possessing a highly developed porosity demonstrate high adsorption capacities. More specifically, carbon cloths show high adsorption rates, an easily handling, a good mechanical integrity and regeneration potentialities. When loaded with pollutants, these materials can be indeed regenerated using an electrochemical polarization.

Keywords: nanoporous carbons, activated carbon cloths, adsorption, micropollutants, emerging contaminants, regeneration, electrochemistry

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Authors: Talal Alshammari, Nasser Alshammari, Mohamed Sedky, Chris Howard

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With the widespread adoption of the Internet-connected devices, and with the prevalence of the Internet of Things (IoT) applications, there is an increased interest in machine learning techniques that can provide useful and interesting services in the smart home domain. The areas that machine learning techniques can help advance are varied and ever-evolving. Classifying smart home inhabitants’ Activities of Daily Living (ADLs), is one prominent example. The ability of machine learning technique to find meaningful spatio-temporal relations of high-dimensional data is an important requirement as well. This paper presents a comparative evaluation of state-of-the-art machine learning techniques to classify ADLs in the smart home domain. Forty-two synthetic datasets and two real-world datasets with multiple inhabitants are used to evaluate and compare the performance of the identified machine learning techniques. Our results show significant performance differences between the evaluated techniques. Such as AdaBoost, Cortical Learning Algorithm (CLA), Decision Trees, Hidden Markov Model (HMM), Multi-layer Perceptron (MLP), Structured Perceptron and Support Vector Machines (SVM). Overall, neural network based techniques have shown superiority over the other tested techniques.

Keywords: activities of daily living, classification, internet of things, machine learning, prediction, smart home

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Authors: Camille Perréard, Yoann Ladner, Fanny D'Orlyé, Stéphanie Descroix, Vélan Taniga, Anne Varenne, Cédric Guyon, Michael. Tatoulian, Frédéric Kanoufi, Cyrine Slim, Sophie Griveau, Fethi Bedioui

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The development of micro total analysis systems is of major interest for contaminant and biomarker analysis. As a lab-on-chip integrates all steps of an analysis procedure in a single device, analysis can be performed in an automated format with reduced time and cost, while maintaining performances comparable to those of conventional chromatographic systems. Moreover, these miniaturized systems are either compatible with field work or glovebox manipulations. This work is aimed at developing an analytical microsystem for trace and ultra trace quantitation in complex matrices. The strategy consists in the integration of a sample pretreatment step within the lab-on-chip by a confinement zone where selective ligands are immobilized for target extraction and preconcentration. Aptamers were chosen as selective ligands, because of their high affinity for all types of targets (from small ions to viruses and cells) and their ease of synthesis and functionalization. This integrated target extraction and concentration step will be followed in the microdevice by an electrokinetic separation step and an on-line detection. Polymers consisting of cyclic olefin copolymer (COC) or fluoropolymer (Dyneon THV) were selected as they are easy to mold, transparent in UV-visible and have high resistance towards solvents and extreme pH conditions. However, because of their low chemical reactivity, surface treatments are necessary. For the design of this miniaturized diagnostics, we aimed at modifying the microfluidic system at two scales : (1) on the entire surface of the microsystem to control the surface hydrophobicity (so as to avoid any sample wall adsorption) and the fluid flows during electrokinetic separation, or (2) locally so as to immobilize selective ligands (aptamers) on restricted areas for target extraction and preconcentration. We developed different novel strategies for the surface functionalization of COC and Dyneon, based on plasma, chemical and /or electrochemical approaches. In a first approach, a plasma-induced immobilization of brominated derivatives was performed on the entire surface. Further substitution of the bromine by an azide functional group led to covalent immobilization of ligands through “click” chemistry reaction between azides and terminal alkynes. COC and Dyneon materials were characterized at each step of the surface functionalization procedure by various complementary techniques to evaluate the quality and homogeneity of the functionalization (contact angle, XPS, ATR). With the objective of local (micrometric scale) aptamer immobilization, we developed an original electrochemical strategy on engraved Dyneon THV microchannel. Through local electrochemical carbonization followed by adsorption of azide-bearing diazonium moieties and covalent linkage of alkyne-bearing aptamers through click chemistry reaction, typical dimensions of immobilization zones reached the 50 µm range. Other functionalization strategies, such as sol-gel encapsulation of aptamers, are currently investigated and may also be suitable for the development of the analytical microdevice. The development of these functionalization strategies is the first crucial step in the design of the entire microdevice. These strategies allow the grafting of a large number of molecules for the development of new analytical tools in various domains like environment or healthcare.

Keywords: alkyne-azide click chemistry (CuAAC), electrochemical modification, microsystem, plasma bromination, surface functionalization, thermoplastic polymers

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Authors: Yohann R. J. Thomas, Sébastien Solan

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Conventional battery technology includes the assembly of electrode/separator/electrode by standard techniques such as stacking or winding, depending on the format size. In that type of batteries, coating or pasting techniques are only used for the electrode process. The processes are suited for large scale production of batteries and perfectly adapted to plenty of application requirements. Nevertheless, as the demand for both easier and cost-efficient production modes, flexible, custom-shaped and efficient small sized batteries is rising. Thin-film, printable batteries are one of the key areas for printed electronics. In the frame of European BASMATI project, we are investigating the feasibility of a new design of lithium-ion battery: interdigitated planar core design. Polymer substrate is used to produce bendable and flexible rechargeable accumulators. Direct fully printed batteries lead to interconnect the accumulator with other electronic functions for example organic solar cells (harvesting function), printed sensors (autonomous sensors) or RFID (communication function) on a common substrate to produce fully integrated, thin and flexible new devices. To fulfill those specifications, a high resolution printing process have been selected: Aerosol jet printing. In order to fit with this process parameters, we worked on nanomaterials formulation for current collectors and electrodes. In addition, an advanced printed polymer-electrolyte is developed to be implemented directly in the printing process in order to avoid the liquid electrolyte filling step and to improve safety and flexibility. Results: Three different current collectors has been studied and printed successfully. An ink of commercial copper nanoparticles has been formulated and printed, then a flash sintering was applied to the interdigitated design. A gold ink was also printed, the resulting material was partially self-sintered and did not require any high temperature post treatment. Finally, carbon nanotubes were also printed with a high resolution and well defined patterns. Different electrode materials were formulated and printed according to the interdigitated design. For cathodes, NMC and LFP were efficaciously printed. For anodes, LTO and graphite have shown to be good candidates for the fully printed battery. The electrochemical performances of those materials have been evaluated in a standard coin cell with lithium-metal counter electrode and the results are similar with those of a traditional ink formulation and process. A jellified plastic crystal solid state electrolyte has been developed and showed comparable performances to classical liquid carbonate electrolytes with two different materials. In our future developments, focus will be put on several tasks. In a first place, we will synthesize and formulate new specific nano-materials based on metal-oxyde. Then a fully printed device will be produced and its electrochemical performance will be evaluated.

Keywords: high resolution digital printing, lithium-ion battery, nanomaterials, solid-state electrolytes

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Authors: Zbigniew Szklarz, Aldona Garbacz-Klempka, Magdalena Bisztyga-Szklarz

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Typical metallic alloys bases on one major alloying component, where the addition of other elements is intended to improve or modify certain properties, most of all the mechanical properties. However, in 1995 a new concept of metallic alloys was described and defined. High Entropy Alloys (HEA) contains at least five alloying elements in an amount from 5 to 20 at.%. A common feature this type of alloys is an absence of intermetallic phases, high homogeneity of the microstructure and unique chemical composition, what leads to obtaining materials with very high strength indicators, stable structures (also at high temperatures) and excellent corrosion resistance. Hence, HEA can be successfully used as a substitutes for typical metallic alloys in various applications where a sufficiently high properties are desirable. For fabricating HEA, a few ways are applied: 1/ from liquid phase i.e. casting (usually arc melting); 2/ from solid phase i.e. powder metallurgy (sintering methods preceded by mechanical synthesis) and 3/ from gas phase e.g. sputtering or 4/ other deposition methods like electrodeposition from liquids. Application of different production methods creates different microstructures of HEA, which can entail differences in their properties. The last two methods also allows to obtain coatings with HEA structures, hereinafter referred to as High Entropy Films (HEF). With reference to above, the crucial aim of this work was the optimization of the manufacturing process of the multi-component metallic layers (HEF) by the low- and high temperature electrochemical deposition ( ED). The low-temperature deposition process was crried out at ambient or elevated temperature (up to 100 ᵒC) in organic electrolyte. The high-temperature electrodeposition (several hundred Celcius degrees), in turn, allowed to form the HEF layer by electrochemical reduction of metals from molten salts. The basic chemical composition of the coatings was CoCrFeMnNi (known as Cantor’s alloy). However, it was modified by other, selected elements like Al or Cu. The optimization of the parameters that allow to obtain as far as it possible homogeneous and equimolar composition of HEF is the main result of presented studies. In order to analyse and compare the microstructure, SEM/EBSD, TEM and XRD techniques were employed. Morover, the determination of corrosion resistance of the CoCrFeMnNi(Cu or Al) layers in selected electrolytes (i.e. organic and non-organic liquids) was no less important than the above mentioned objectives.

Keywords: high entropy alloys, electrodeposition, corrosion behavior, microstructure

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Authors: Imtiaz Ahmed Khan, Sabu John, Sania Waqar, Lijing Wang, Mac Fergusson, Ilija Najdovski

Abstract:

Evolution of textiles, from its orthodox to more interactive role has stirred the researchers to uncover its application in numerous arenas. The idea of using textile based materials for wearable energy harvesting and storage devices have gained immense popularity. This is mainly due to textile comfort and flexibility features. In this work, nano-carbonous materials were infused on cellulosic fibers using caustic soda treatment. This paper presents the complete procedure of yarn supercapacitors fabrication process through dip coating technique and its characterization method. The main objective is to study, the effect of varying caustic soda concentration on mass loading of activated carbon on yarns and the related capacitance output of the designed yarn supercapacitor. Polyvinyl alcohol and Phosphoric acid were used as electrolyte in a two-electrode cell assembly to measure device electrochemical performance. The results show a promising increase in capacitance value using this technique.

Keywords: yarn supercapacitors, activated carbon, dip coating, caustic soda, electrolyte, electrochemical characterization

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

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

Keywords: carbon steel, oilfield, corrosion, anionic surfactants

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Authors: V. Sai Geethika, Sai Snehitha Yadavalli, Swati Ghosh Acharyya

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This study involves a single element and simultaneous electrochemical detection of heavy metal ions through square wave anodic stripping voltammetry. A glassy carbon electrode was used to detect and quantify heavy metals such as As(III), Hg(II), Cr(VI) ions in water. Under optimized conditions, peak separation was obtained by varying concentrations, scan rates, and temperatures. As (III), Hg (II), Cr (III) were simultaneously detected with GCE. Several analytical methods, such as inductively coupled plasma mass spectroscopy (ICP-MS), atomic absorption spectroscopy (AAS), were used previously to detect heavy metal ions, which are authentic but are not good enough for online monitoring due to the bulkiness of the equipment. The study provides a good alternative that is simple, more efficient, and low-cost, involving a portable potentiostat. Heavy metals having different oxidation states can be detected by anodic stripping voltammetry. This method can be easily integrated with electronics. Square wave Anodic stripping voltammetry is used with a potential range of -2.5 V – 2.5 V for single ion detection by a three-electrode cell consisting of silver/silver chloride(Ag/AgCl) as reference and platinum (Pt) counter and glassy carbon (GCE) working electrodes. All three ions are optimized by varying the parameters like concentration, scan rate, pH, temperature, and all these optimized parameters were used for studying the effects of simultaneous detection. The procedure involves preparing an electrolyte using deionized water, cleaning the surface of GCE, depositing the ions by applying the redox potentials obtained from cyclic voltammetry (CV), and then detecting by applying oxidizing potential, i.e., stripping voltage. So this includes ASV techniques such as open-circuit voltage (OCV), chronoamperometry (CA), and square wave voltammetry (SWV). Firstly, the concentration of the ions varied from 50 ppb to 5000 ppb, and an optimum concentration was determined where the three ions were detected. A concentration of 400 ppb was used while varying the temperatures in the range of 25°C – 45°C. Optimum peak intensity was obtained at a temperature of 30°C with a low scan rate of 0.005 V-s⁻¹. All the parameters were optimized, and several effects have been noticed while three ions As(II), Cr(III), Hg(II) were detected alone and simultaneously.

Keywords: Arsenic(III), Chromium(III), glassy carbon electrode, Mercury (II), square wave anodic stripping voltammetry

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Authors: Abdi Djamila, Haffar Hichem

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

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

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Authors: Wei Quan, Liu Chao, Mohammed N. Afsar

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The dielectric properties and ionic conductivity of novel "ceramic state" polymer electrolytes for high capacity lithium battery are characterized by radio-frequency and Microwave methods in two broad frequency ranges from 50 Hz to 20 KHz and 4 GHz to 40 GHz. This innovative solid polymer electrolyte which is highly ionic conductive (10-3 S/cm at room temperature) from -40 oC to +150 oC and can be used in any battery application. Such polymer exhibits properties more like a ceramic rather than polymer. The various applied measurement methods produced accurate dielectric results for comprehensive analysis of electrochemical properties and ion transportation mechanism of this newly invented polymer electrolyte. Two techniques and instruments employing air gap measurement by capacitance bridge and inwave guide measurement by vector network analyzer are applied to measure the complex dielectric spectra. The complex dielectric spectra are used to determine the complex alternating current electrical conductivity and thus the ionic conductivity.

Keywords: polymer electrolyte, dielectric permittivity, lithium battery, ionic relaxation, microwave measurement

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Authors: Mai M. Khalaf, Hany M. Abd El-Lateef

Abstract:

A new good application for the sol gel method is to improve the corrosion inhibition properties of carbon steel by the dip coating method of Nano TiO2 films and its modification with Poly Ethylene Glycol (PEG). The prepared coating samples were investigated by different techniques, X-ray diffraction, Scanning Electron Microscopy (SEM), transmission electron microscopy and Energy Dispersive X-ray Spectroscopy (EDAX). The corrosion inhibition performance of the blank carbon steel and prepared coatings samples were evaluated in 0.5 M H2SO4 by using Electrochemical Impedance Spectroscopy (EIS) and potentiodynamic polarization measurements. The results showed that corrosion resistance of carbon steel increases with increasing the number of coated layers of both nano–TiO2 films and its modification of PEG. SEM-EDAX analyses confirmed that the percentage atomic content of iron for the carbon steel in 0.5 M H2SO4 is 83% and after the deposition of the steel in nano TiO2 sol and that with PEG are 94.3% and 93.7% respectively.

Keywords: dip-coatings, corrosion protection, sol gel, TiO2 films, PEG

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