Search results for: scanning electrochemical microscopy

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: Aisha Ganash

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Poly(o-phenylendiamine) and poly(ophenylendiamine)/ZnO(PoPd/ZnO) nanocomposites coating were prepared on type-304 austenitic stainless steel (SS) using H2SO4 acid as electrolyte by potentiostatic methods. Fourier transforms infrared spectroscopy and scanning electron microscopy techniques were used to characterize the composition and structure of PoPd/ZnO nanocomposites. The corrosion protection of polymer coatings ability was studied by Eocp-time measurement, anodic and cathodic potentiodynamic polarization and Impedance techniques in 3.5% NaCl as a corrosive solution. It was found that ZnO nanoparticles improve the barrier and electrochemical anticorrosive properties of poly(o-phenylendiamine).

Keywords: anticorrosion, conducting polymers, electrochemistry, nanocomposites

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Authors: Ozan Kahraman, Hao Feng

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Manothermosonication (MTS), which consists of the simultaneous application of heat and ultrasound under moderate pressure (100-700 kPa), is one of the technologies which destroy microorganisms and inactivates enzymes. Transmission electron microscopy (TEM) is a microscopy technique in which a beam of electrons is transmitted through an ultra-thin specimen, interacting with the specimen as it passes through it. The environmental scanning electron microscope or ESEM is a scanning electron microscope (SEM) that allows for the option of collecting electron micrographs of specimens that are "wet," uncoated. These microscopy techniques allow us to observe the processing effects on the samples. This study was conducted to investigate the effects of MTS and HTST treatments on the morphology of apple-carrot juices by using TEM and ESEM microscopy. Apple-carrot juices treated with HTST (72 0C, 15 s), MTS 50 °C (60 s, 200 kPa), and MTS 60 °C (30 s, 200 kPa) were observed in both ESEM and TEM microscopy. For TEM analysis, a drop of the solution dispersed in fixative solution was put onto a Parafilm ® sheet. The copper coated side of the TEM sample holder grid was gently laid on top of the droplet and incubated for 15 min. A drop of a 7% uranyl acetate solution was added and held for 2 min. The grid was then removed from the droplet and allowed to dry at room temperature and presented into the TEM. For ESEM analysis, a critical point drying of the filters was performed using a critical point dryer (CPD) (Samdri PVT- 3D, Tousimis Research Corp., Rockville, MD, USA). After the CPD, each filter was mounted onto a stub and coated with gold/palladium with a sputter coater (Desk II TSC Denton Vacuum, Moorestown, NJ, USA). E.Coli O157:H7 cells on the filters were observed with an ESEM (Philips XL30 ESEM-FEG, FEI Co., Eindhoven, The Netherland). ESEM (Environmental Scanning Electron Microscopy) and TEM (Transmission Electron Microscopy) images showed extensive damage for the samples treated with MTS at 50 and 60 °C such as ruptured cells and breakage on cell membranes. The damage was increasing with increasing exposure time.

Keywords: MTS, HTST, ESEM, TEM, E.COLI O157:H7

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Authors: S. Mohajeri

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Electrocodeposition of Ni-TiO2 nanocomposite single layers and Ni-TiO2/TiO2 multilayers from Watts bath containing TiO2 sol was carried out on copper substrate. Pulse plating and pulse reverse plating techniques were applied to facilitate higher incorporations of TiO2 nanoparticles in Ni-TiO2 nanocomposite single layers, and the results revealed that by prolongation of the current-off durations and the anodic cycles, deposits containing 11.58 wt.% and 13.16 wt.% TiO2 were produced, respectively. Multilayer coatings which consisted of Ni-TiO2 and TiO2-rich layers were deposited by pulse potential deposition through limiting the nickel deposition by diffusion control mechanism. The TiO2-rich layers thickness and accordingly, the content of TiO2 reinforcement reached 104 nm and 18.47 wt.%, respectively in the optimum condition. The phase structure and surface morphology of the nanocomposite coatings were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The cross sectional morphology and line scans of the layers were studied by field emission scanning electron microscopy (FESEM). It was confirmed that the preferred orientations and the crystallite sizes of nickel matrix were influenced by the deposition technique parameters, and higher contents of codeposited TiO2 nanoparticles refined the microstructure. The corrosion behavior of the coatings in 1M NaCl and 0.5M H2SO4 electrolytes were compared by means of potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) techniques. Increase of corrosion resistance and the passivation tendency were favored by TiO2 incorporation, while the degree of passivation declined as embedded particles disturbed the continuity of passive layer. The role of TiO2 incorporation on the improvement of mechanical properties including hardness, elasticity, scratch resistance and friction coefficient was investigated by the means of atomic force microscopy (AFM). Hydrophilicity and wettability of the composite coatings were investigated under UV illumination, and the water contact angle of the multilayer was reduced to 7.23° after 1 hour of UV irradiation.

Keywords: electrodeposition, hydrophilicity, multilayer, pulse-plating

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Authors: Seyda Tugba Gunday Anil, Ayhan Bozkurt

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Next generation lithium batteries are taking more attention and single-ion polymer electrolytes are expected to play a significant role in the development of these kinds of energy storage systems. In the present work we used a different strategy to design of novel solid single-ion conducting inorganic polymer electrolytes based on lithium polyvinyl alcohol oxalate borate (Li(PVAOB), lithium polyacrylic acid oxalate borate (LiPAAOB) and poly (ethylene glycol) methacrylate (PEGMA). Free radical polymerization was used to convert PEGMA into PPEGMA and LiPAAOB is prepared from poly (acrylic acid), oxalic acid and boric acid. Blend polymer electrolytes were produced by mixing of LiPAAOB or Li (PVAOB with PPEGMA at different stoichiometric ratios to enhance the single ion conductivity of the systems. To exploit the flexible chemistry and increase the segmental mobility of the blend electrolyte, the composition was changed up to 80% with respect to the guest polymer, PPEGMA. FT-IR and differential scanning calorimeter techniques confirmed the interaction between the host and guest polymers. TGA verified that the thermal stability of the blends increased up to approximately 200 C. Scanning electron microscopy images confirm the homogeneity of the blend electrolytes. CV studies showed that electrochemical stability electrochemical stability window is approximately 5 V versus Li/Li⁺. The effect of PPEGMA on to the Lithium-ion conductivity was investigated using dielectric impedance analyzer. The maximum single ion conductivity was measured as 1.3 × 10⁻⁴ S/cm at 100 C for the sample LiPAAOB-80PPEGMA. Clearly, the results confirmed the positive effect to the increment in ionic conductivity of the blend electrolytes with the addition of PPEGMA.

Keywords: single-ion conductor, inorganic polymer, blends, polymer electrolyte

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Authors: Adil Tamimi

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Limestone powder is a natural material that is available in many parts of the world. In this research self-compacting concrete was designed and prepared using limestone powder. The resulted concrete was exposed to the hydrochloric acid solution and compared with reference concrete. Mechanical properties of both fresh and hardened concrete have been evaluated. Scanning Electron Microscopy “SEM” has been unitized to analyse the morphological development of the hydration products. In sulphuric acid solution, a large formation of gypsum was detected in both samples of self-compacting concrete and conventional concrete. The Higher amount of thaumasite and ettringite was also detected in the SCC sample. In hydrochloric acid solution, monochloroaluminate was detected.

Keywords: self-compacting concrete, mechanical properties, Scanning Electron Microscopy, acid solution

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Authors: Sharan K. Indrakar, Aakash B. Prasad, Arash Takshi, Sesha Srinivasan, Elias K. Stefanakos

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In this work, we present an exclusive study on the effect of the feeding ratio of polyaniline-based redox-active gel layer on electrical and optical properties of innovative electrochromic devices (ECs). An electrochromic device consisting of polyaniline (PANI) has a redox-active gel electrolyte placed between two conducting transparent fluorine-doped tin oxide glass substrates. The redox-active composite gel is a mixture of different concentrations of aniline (monomer), a water-soluble polymer poly (vinyl alcohol), hydrochloric acid, and an oxidant. The EC device shows the color change from dark green to transparent for the applied potential between -0.5 V to +2.0 V. The coloration and decoloration of the ECs were tested for electrochemical behavior using techniques such as cyclic voltammetry (CV), chronoamperometry (CA), and electrochemical impedance spectroscopy (EIS). The optical transparency of the EC devices was examined at two different biasing voltage conditions under UV-visible spectroscopic technique; the result showed 65% transmittance at 564 nm and zero transmittance when the cell was biased at 0.0 V and 2.0 V, the synthesized mol fraction gel was analyzed for surface morphology and structural properties by scanning electron microscopy and Fourier transformer spectroscopy.

Keywords: electrochromic, gel electrolyte, polyaniline, conducting polymer

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Authors: Rehan Deshmukh, Sunil Bhand, Utpal Roy

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We report the label-free electrochemical detection of Escherichia coli O157:H7 (ATCC 43895) in potable water using a DNA probe as a sensing molecule targeting the open reading frame marker. Indium tin oxide (ITO) surface was modified with organosilane and, glutaraldehyde was applied as a linker to fabricate the DNA sensor chip. Non-Faradic electrochemical impedance spectroscopy (EIS) behavior was investigated at each step of sensor fabrication using cyclic voltammetry, impedance, phase, relative permittivity, capacitance, and admittance. Atomic force microscopy (AFM) and scanning electron microscopy (SEM) revealed significant changes in surface topographies of DNA sensor chip fabrication. The decrease in the percentage of pinholes from 2.05 (Bare ITO) to 1.46 (after DNA hybridization) suggested the capacitive behavior of the DNA sensor chip. The results of non-Faradic EIS studies of DNA sensor chip showed a systematic declining trend of the capacitance as well as the relative permittivity upon DNA hybridization. DNA sensor chip exhibited linearity in 0.5 to 25 pg/10mL for E. coli O157:H7 (ATCC 43895). The limit of detection (LOD) at 95% confidence estimated by logistic regression was 0.1 pg DNA/10mL of E. coli O157:H7 (equivalent to 13.67 CFU/10mL) with a p-value of 0.0237. Moreover, the fabricated DNA sensor chip used for detection of E. coli O157:H7 showed no significant cross-reactivity with closely and distantly related bacteria such as Escherichia coli MTCC 3221, Escherichia coli O78:H11 MTCC 723 and Bacillus subtilis MTCC 736. Consequently, the results obtained in our study demonstrated the possible application of developed DNA sensor chips for E. coli O157:H7 ATCC 43895 in real water samples as well.

Keywords: capacitance, DNA sensor, Escherichia coli O157:H7, open reading frame marker

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Authors: N. I. Kargin, G. K. Safaraliev, A. S. Gusev, A. O. Sultanov, N. V. Siglovaya, S. M. Ryndya, A. A. Timofeev

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In this paper, an experimental and theoretical study of the processes of mesoporous silicon carbonization during the formation of buffer layers for the subsequent epitaxy of 3C-SiC films and related wide-band-gap semiconductors is performed. Experimental samples were obtained by the method of chemical vapor deposition and investigated by scanning electron microscopy. Analytic expressions were obtained for the effective diffusion factor and carbon atoms diffusion length in a porous system. The proposed model takes into account the processes of Knudsen diffusion, coagulation and overgrowing of pores during the formation of a silicon carbide layer.

Keywords: silicon carbide, porous silicon, carbonization, electrochemical etching, diffusion

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Authors: Hany M. Abd El-Lateef

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

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

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

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

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

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Authors: Manuel Salado, Mikel Rincón, Arkaitz Fidalgo, Roberto Fernandez, Senentxu Lanceros-Méndez

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Lithium-ion batteries (LIBs) are a promising technology for energy storage, but they suffer from safety concerns due to the use of flammable organic solvents in their liquid electrolytes. Solid-state electrolytes (SSEs) offer a potential solution to this problem, but they have their own limitations, such as poor ionic conductivity and high interfacial resistance. The aim of this research was to develop a new type of SSE based on metal-organic frameworks (MOFs) and ionic liquids (ILs). MOFs are porous materials with high surface area and tunable electronic properties, making them ideal for use in SSEs. ILs are liquid electrolytes that are non-flammable and have high ionic conductivity. A series of MOFs were synthesized, and their electrochemical properties were evaluated. The MOFs were then infiltrated with ILs to form a quasi-solid gel and solid xerogel SSEs. The ionic conductivity, interfacial resistance, and electrochemical performance of the SSEs were characterized. The results showed that the MOF-IL SSEs had significantly higher ionic conductivity and lower interfacial resistance than conventional SSEs. The SSEs also exhibited excellent electrochemical performance, with high discharge capacity and long cycle life. The development of MOF-IL SSEs represents a significant advance in the field of solid-state electrolytes. The high ionic conductivity and low interfacial resistance of the SSEs make them promising candidates for use in next-generation LIBs. The data for this research was collected using a variety of methods, including X-ray diffraction, scanning electron microscopy, and electrochemical impedance spectroscopy. The data was analyzed using a variety of statistical and computational methods, including principal component analysis, density functional theory, and molecular dynamics simulations. The main question addressed by this research was whether MOF-IL SSEs could be developed that have high ionic conductivity, low interfacial resistance, and excellent electrochemical performance. The results of this research demonstrate that MOF-IL SSEs are a promising new type of solid-state electrolyte for use in LIBs. The SSEs have high ionic conductivity, low interfacial resistance, and excellent electrochemical performance. These properties make them promising candidates for use in next-generation LIBs that are safer and have higher energy densities.

Keywords: energy storage, solid-electrolyte, ionic liquid, metal-organic-framework, electrochemistry, organic inorganic plastic crystal

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Authors: Ifeyinwa Orakwe, Ngozi Nwogu, Edward Gobina

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This work presents experimental results relating to the structural characterization of a commercially available alumina membrane. A γ-alumina mesoporous tubular membrane has been used. Nitrogen adsorption-desorption, scanning electron microscopy and gas permeability test has been carried out on the alumina membrane to characterize its structural features. Scanning electron microscopy (SEM) was used to determine the pore size distribution of the membrane. Pore size, specific surface area and pore size distribution were also determined with the use of the Nitrogen adsorption-desorption instrument. Gas permeation tests were carried out on the membrane using a variety of single and mixed gases. The permeabilities at different pressure between 0.05-1 bar and temperature range of 25-200oC were used for the single and mixed gases: nitrogen (N2), helium (He), oxygen (O2), carbon dioxide (CO2), 14%CO₂/N₂, 60%CO₂/N₂, 30%CO₂/CH4 and 21%O₂/N₂. Plots of flow rate verses pressure were obtained. Results got showed the effect of temperature on the permeation rate of the various gases. At 0.5 bar for example, the flow rate for N2 was relatively constant before decreasing with an increase in temperature, while for O2, it continuously decreased with an increase in temperature. In the case of 30%CO₂/CH4 and 14%CO₂/N₂, the flow rate showed an increase then a decrease with increase in temperature. The effect of temperature on the membrane performance of the various gases is presented and the influence of the trans membrane pressure drop will be discussed in this paper.

Keywords: alumina membrane, Nitrogen adsorption-desorption, scanning electron microscopy, gas permeation, temperature

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Authors: Kathleen Moyer, Nora Ait Boucherbil, Murtaza Zohair, Janna Eaves-Rathert, Cary Pint

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This study demonstrates the significance of interface engineering in the field of structural energy by being the first case where the performance of the system with the structural battery is greater than the performance of the same system with a battery separate from the system. The benefits of improving the interface in the structural battery were tested by creating carbon fiber composite batteries (and independent graphite electrodes and lithium iron phosphate electrodes) with and without an improved interface. Mechanical data on the structural batteries were collected using tensile tests and electrochemical data was collected using scanning electron microscopy equipment. The full-cell lithium-ion structural batteries had capacity retention of over 80% exceeding 100 cycles with an average energy density of 52 W h kg−1 and a maximum energy density of 58 W h kg−1. Most scientific developments in the field of structural energy have been done with supercapacitors. Most scientific developments with structural batteries have been done where batteries are simply incorporated into the structural element. That method has limited advantages and can create mechanical disadvantages. This study aims to show that a large improvement in structure energy research can be made by improving the interface between the structural device and the battery.

Keywords: composite materials, electrochemical performance, mechanical properties, polymer interface, structural batteries

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Authors: Irshad U. Khan, Tanmay Paul, Murali Mohan Seepana

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This paper presents a study on synthesizing and characterizing a Copper oxide doped Carbon (CuO-C) electrocatalyst for the negative half-cell reactions of Vanadium Redox Flow Battery (VRFB). The CuO was synthesized using a microreactor. The electrocatalyst was characterized using X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and Field Emission Scanning Electron Microscopy (SEM). The electrochemical performance was assessed by linear sweep voltammetry (LSV). The findings suggest that the synthesized CuO exhibited favorable crystallinity, morphology, and surface area, which reflects improved cell performance.

Keywords: ECSA, electrocatalyst, energy storage, Tafel

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Authors: Hilal Kivrak, Aykut ÇağLar, Nahit Aktaş, Ali Osman Solak

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At present, Cd/TiO₂ and CdTe/TiO₂ catalysts are prepared via sodium borohydride (NaBH4) reduction method. These catalysts are characterized by fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). These Cd/TiO₂ and CdTe/TiO₂ are employed as catalysts for the photocatalytic oxidation of glucose. Cyclic voltammetry (CV), chronoamperometry (CA), and electrochemical impedance spectroscopy (EIS) measurements are used to investigate their glucose electrooxidation activities of catalysts at long and under UV illumination (ʎ=354 nm). CdTe/TiO₂ catalyst is showed the best photocatalytic glucose electrooxidation activity compared to Cd/TiO₂ catalyst.

Keywords: cadmium, NaBH4 reduction method, photocatalytic glucose electrooxidation, Tellerium, TiO2

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Authors: Anju Joshi, C. N. Tharamani

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

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

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Authors: Roaa Sait, Richard Cross

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The synthesis and characterization of one dimensional nanostructure such as nanowires has received considerable attention. Much effort has concentrated on TiN material especially in the biological field due to its useful and unique properties in this field. Therefore, for the purpose of this project, synthesis of Titanium Nitride (TiN) nanowires (NWs) will be presented. They will be synthesised by growing titanium dioxide (Ti) NWs in an aqueous solution at low temperatures under atmospheric pressure. Then the grown nanowires will undergo a 'Nitrodation process' in which results in the formation of TiN NWs. The structure, morphology and composition of the grown nanowires will be characterized using Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), X-ray Diffraction (XRD) and Cyclic Voltammetry (CV). Obtaining TiN NWs is a challenging task since it has not been formulated before, as far as we acknowledge. This might be due to the fact that nitriding Ti NWs can be difficult in terms of optimizing experimental parameters.

Keywords: nanowires, dissolution-growth, nucleation, PECVD, deposition, spin coating, scanning electron microscopic analysis, cyclic voltammetry analysis

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

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

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

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Authors: Hubert Beisch, Janik Marx, Svenja Garlof, Roman Shvets, Ivan Grygorchak, Andriy Kityk, Bodo Fiedler

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Three-dimensional carbon materials can be used as electrode materials for energy storage systems such as batteries and supercapacitors. Fast charging and discharging times are realizable without reducing the performance due to aging processes. Furthermore high specific surface area (SSA) of three-dimensional carbon structures leads to high specific capacities. One newly developed carbon foam is Globugraphite. This interconnected globular carbon morphology with statistically distributed hierarchical pores is manufactured by a chemical vapor deposition (CVD) process from ceramic templates resulting from a sintering process. Via scanning electron (SEM) and transmission electron microscopy (TEM), the morphology is characterized. Moreover, the SSA was measured by the Brunauer–Emmett–Teller (BET) theory. Measurements of Globugraphite in an organic and inorganic electrolyte show high energy densities and power densities resulting from ion absorption by forming an electrochemical double layer. A comparison of the specific values is summarized in a Ragone diagram. Energy densities up to 48 Wh/kg and power densities to 833 W/kg could be achieved for an SSA from 376 m²/g to 859 m²/g. For organic electrolyte, a specific capacity of 100 F/g at a density of 20 mg/cm³ was achieved.

Keywords: BET, carbon foam, CVD process, electrochemical cell, Ragone diagram, SEM, TEM

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Authors: Bing–Jing Zhao, Chang-Kui Liu, Hong Wang, Min Hu

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Electron beam rapid manufacturing (EBRM) or Selective laser melting is an additive manufacturing process that uses 3D CAD data as a digital information source and energy in the form of a high-power laser beam or electron beam to create three-dimensional metal parts by fusing fine metallic powders together.Object:The present study was conducted to evaluate the mechanical properties ,the phase transformation,the corrosivity and the biocompatibility of Ti-6Al-4V by EBRM,SLM and forging technique.Method: Ti-6Al-4V alloy standard test pieces were manufactured by EBRM, SLM and forging technique according to AMS4999,GB/T228 and ISO 10993.The mechanical properties were analyzed by universal test machine. The phase transformation was analyzed by X-ray diffraction and scanning electron microscopy. The corrosivity was analyzed by electrochemical method. The biocompatibility was analyzed by co-culturing with mesenchymal stem cell and analyzed by scanning electron microscopy (SEM) and alkaline phosphatase assay (ALP) to evaluate cell adhesion and differentiation, respectively. Results: The mechanical properties, the phase transformation, the corrosivity and the biocompatibility of Ti-6Al-4V by EBRM、SLM were similar to forging and meet the mechanical property requirements of AMS4999 standard. a­phase microstructure for the EBM production contrast to the a’­phase microstructure of the SLM product. Mesenchymal stem cell adhesion and differentiation were well. Conclusion: The property of the Ti-6Al-4V alloy manufactured by EBRM and SLM technique can meet the medical standard from this study. But some further study should be proceeded in order to applying well in clinical practice.

Keywords: 3D printing, Electron Beam Rapid Manufacturing (EBRM), Selective Laser Melting (SLM), Computer Aided Design (CAD)

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Authors: Umran Kurtan, Hamide Aydin, Sevim Unugur Celik, Ayhan Bozkurt

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In the present work, novel hBN/polyacrylonitrile composite nanofibers were produced via electrospinning approach and loaded with the electrolyte for rechargeable lithium-ion battery applications. The electrospun nanofibers comprising various hBN contents were characterized by using Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. The influence of hBN/PAN ratios onto the properties of the porous composite system, such as fiber diameter, porosity, and the liquid electrolyte uptake capability were systematically studied. Ionic conductivities and electrochemical characterizations were evaluated after loading electrospun hBN/PAN composite nanofiber with liquid electrolyte, i.e., 1 M lithium hexafluorophosphate (LiPF6) in ethylene carbonate (EC)/ethyl methyl carbonate (EMC) (1:1 vol). The electrolyte loaded nanofiber has a highest ionic conductivity of 10−3 S cm⁻¹ at room temperature. According to cyclic voltammetry (CV) results it exhibited a high electrochemical stability window up to 4.7 V versus Li+/Li. Li//10 wt% hBN/PAN//LiCO₂ cell was produced which delivered high discharge capacity of 144 mAhg⁻¹ and capacity retention of 92.4%. Considering high safety and low cost properties of the resulting hBN/PAN fiber electrolytes, these materials can be suggested as potential separator materials for lithium-ion batteries.

Keywords: hexagonal boron nitride, polyacrylonitrile, electrospinning, lithium ion battery

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Authors: M. F. Perez, Ysmael Verde, B. Escobar, R. Barbosa, J. C. Cruz

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Reinforced concrete is one of the most important materials in the construction industry. However, in recent years the durability of concrete structures has been a worrying problem, mainly due to corrosion of reinforcing steel; the consequences of corrosion in all cases lead to shortening of the life of the structure and decrease in quality of service. Since the emergence of this problem, they have implemented different methods or techniques to reduce damage by corrosion of reinforcing steel in concrete structures; as the use of polymeric materials as coatings for the steel rod, spiked inhibitors of concrete during mixing, among others, presenting different limitations in the application of these methods. Because of this, it has been used a method that has proved effective, cathodic protection. That is why due to the properties attributed to carbon nanotubes (CNT), these could act as cathodic corrosion protection. Mounting a three-electrode electrochemical cell, carbon steel as working electrode, saturated calomel electrode (SCE) as the reference electrode, and a graphite rod as a counter electrode to close the system is performed. Samples made were subjected to a cycling process in order to compare the results in the corrosion performance of a coating composed of CNT and the others based on an anticorrosive commercial painting. The samples were tested at room temperature using an electrolyte consisting NaCl and NaOH simulating the typical pH of concrete, ranging from 12.6 to 13.9. Three test samples were made of steel rod, white, with commercial anticorrosive paint and CNT based coating; delimiting the work area to a section of 0.71 cm2. Tests cyclic voltammetry and linear voltammetry electrochemical spectroscopy each impedance of the three samples were made with a window of potential vs SCE 0.7 -1.7 a scan rate of 50 mV / s and 100 mV / s. The impedance values were obtained by applying a sine wave of amplitude 50 mV in a frequency range of 100 kHz to 100 MHz. The results obtained in this study show that the CNT based coating applied to the steel rod considerably decreased the corrosion rate compared to the commercial coating of anticorrosive paint, because the Ecorr was passed increase as the cycling process. The samples tested in all three cases were observed by light microscopy throughout the cycling process and micrographic analysis was performed using scanning electron microscopy (SEM). Results from electrochemical measurements show that the application of the coating containing carbon nanotubes on the surface of the steel rod greatly increases the corrosion resistance, compared to commercial anticorrosive coating.

Keywords: anticorrosive, carbon nanotubes, corrosion, steel

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Authors: M. El Hajji, A. Hallaoui, L. Bazzi, A. Benlhachemi, Lh. Bazzi, M. Hilali, O. Jbara, A. Tara, B. Bakiz

Abstract:

The cathodic electro deposition of the cuprite Cu2O by chrono potentiometry is performed on two types of electrodes "titanium and stainless steel", in a basic medium containing the precursor of copper. The plot produced vs SCE, shows the formation of a brown layer on the electrode surface. The chrono potentiometric recording made between - 0.2 and - 1 mA/cm2, has allowed us to have a deposit having different morphologies and structural orientation obtained as a function of the variation of many parameters. The morphology, the size of crystals, and the phase of the deposits produced were studied by conventional techniques of analysis of the solid, particularly the X-ray diffraction (XRD), scanning electron microscopy analysis (SEM) and quantitative chemical analysis (EDS). The results will be presented and discussed, they show that the majority of deposits are pure and uniform.

Keywords: cathodic electrodeposition, cuprite Cu2O, XRD, SEM, EDS analysis

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Authors: Theo H. G. Moundzounga

Abstract:

Arsenic and 2-chlorophenol are priority pollutants that pose serious health threats to humans and ecology. An electrochemical sensor, based on graphitic carbon nitride (g-C₃N₄) and carbon dots (CDs), was fabricated and used for the determination of arsenic and 2-chlorophenol. The g-C₃N₄/CDs nanocomposite was prepared via microwave irradiation heating method and was dropped-dried on the surface of the glassy carbon electrode (GCE). Transmission electron microscopy (TEM), X-ray diffraction (XRD), photoluminescence (PL), Fourier transform infrared spectroscopy (FTIR), UV-Vis diffuse reflectance spectroscopy (UV-Vis DRS) were used for the characterization of structure and morphology of the nanocomposite. Electrochemical characterization was done by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The electrochemical behaviors of arsenic and 2-chlorophenol on different electrodes (GCE, CDs/GCE, and g-C₃N₄/CDs/GCE) was investigated by differential pulse voltammetry (DPV). The results demonstrated that the g-C₃N₄/CDs/GCE significantly enhanced the oxidation peak current of both analytes. The analytes detection sensitivity was greatly improved, suggesting that this new modified electrode has great potential in the determination of trace level of arsenic and 2-chlorophenol. Experimental conditions which affect the electrochemical response of arsenic and 2-chlorophenol were studied, the oxidation peak currents displayed a good linear relationship to concentration for 2-chlorophenol (R²=0.948, n=5) and arsenic (R²=0.9524, n=5), with a linear range from 0.5 to 2.5μM for 2-CP and arsenic and a detection limit of 2.15μM and 0.39μM respectively. The modified electrode was used to determine arsenic and 2-chlorophenol in spiked tap and effluent water samples by the standard addition method, and the results were satisfying. According to the measurement, the new modified electrode is a good alternative as chemical sensor for determination of other phenols.

Keywords: electrochemistry, electrode, limit of detection, sensor

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Authors: Giulio Rosati, Luciano Sappia, Rossana Madrid, Noemi Rozlòsnik

Abstract:

The addition of PEG of different molecular weights has important effects on the physical, electrical and electrochemical properties of iron(III)-tosylate doped PEDOT. This particular polymer can be easily spin coated over plastic discs, optimizing thickness and uniformity of the PEDOT-PEG films. The conductivity and morphological analysis of the hybrid PEDOT-PEG polymer by 4-point probe (4PP), 12-point probe (12PP), and conductive AFM (C-AFM) show strong effects of the PEG doping. Moreover, the conductive films kinetics at the nanoscale, in response to different bias voltages, change radically depending on the PEG molecular weight. The hybrid conductive films show also interesting electrochemical properties, making the PEDOT PEG doping appealing for biosensing applications both for EIS-based and amperometric affinity/catalytic biosensors.

Keywords: atomic force microscopy, biosensors, four-point probe, nano-films, PEDOT

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Authors: Abebe Taye

Abstract:

The interest in enhancing the performance of all-solid-state batteries featuring lithium metal anodes as a potential alternative to traditional lithium-ion batteries has prompted exploration into new avenues. A promising strategy involves transforming lithium-ion batteries into hybrid configurations by integrating lithium-ion and lithium-metal solid-state components. This study is focused on achieving stable lithium deposition and advancing the electrochemical capabilities of solid-state lithium hybrid batteries with anodes by incorporating mesocarbon microbeads (MCMBs) blended with silver nanoparticles. To achieve this, mesocarbon microbeads (MCMBs) blended with silver nanoparticles are coated on stainless-steel current collectors. These samples undergo a battery of analyses employing diverse techniques. Surface morphology is studied through scanning electron microscopy (SEM). The electrochemical behavior of the coated samples is evaluated in both half-cell and full-cell setups utilizing an argyrodite-type sulfide electrolyte. The stability of MCMBs in the electrolyte is assessed using electrochemical impedance spectroscopy (EIS). Additional insights into the composition are gleaned through X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and energy-dispersive X-ray spectroscopy (EDS). At an ultra-low N/P ratio of 0.26, stability is upheld for over 100 charge/discharge cycles in half-cells. When applied in a full-cell configuration, the hybrid anode preserves 60.1% of its capacity after 80 cycles at 0.3 C under a low N/P ratio of 0.45. In sharp contrast, the capacity retention of the cell using untreated MCMBs declines to 20.2% after a mere 60 cycles. The introduction of mesocarbon microbeads (MCMBs) combined with silver nanoparticles into the hybrid anode of solid-state lithium batteries substantially elevates their stability and electrochemical performance. This approach ensures consistent lithium deposition and removal, mitigating dendrite growth and the accumulation of inactive lithium. The findings from this investigation hold significant value in elevating the reversibility and energy density of lithium-ion batteries, thereby making noteworthy contributions to the advancement of more efficient energy storage systems.

Keywords: MCMB, lithium metal, hybrid anode, silver nanoparticle, cycling stability

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Authors: Bryan D. Llenarizas, Maria Carla F. Manzano

Abstract:

The rapid growth of electricity demand has led to a pursuit of alternative energy sources with high power output and not harmful to the environment. The fuel cell is a device that generates electricity via chemical reactions between the fuel and oxidant. Fuel cells have been known for decades, but the development of high-power output and durability was still one of the drawbacks of this energy source. This study investigates the potential of layer-by-layer composite for fuel cell applications. A two-electrode electrochemical cell was used for the galvanostatic electrochemical deposition method to fabricate a Polypyrrole/rGO|Polypyrrole/ZnO layer-by-layer composite material for fuel cell applications. In the synthesis, the first layer comprised 0.1M pyrrole monomer and 1mg of rGO, while the second layer had 0.1M pyrrole monomer and variations of ZnO concentration ranging from 0.08M up to 0.12M. A constant current density of 8mA/cm² was applied for 1 hour in fabricating each layer. Scanning electron microscopy (SEM) for the fabricated LBL material shows a globular surface with white spots. These white spots are the ZnO particles confirmed by energy-dispersive X-ray spectroscopy, indicating a successful deposition of the second layer onto the first layer. The observed surface morphology was consistent for each variation of ZnO concentrations. AC measurements were conducted to obtain the AC resistance of the fabricated film. Results show a decrease in AC resistance as the concentration of ZnO increases.

Keywords: anode, composite material, electropolymerization, fuel cell, galvanostatic, polypyrrole

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Authors: Khamael Abualnaja, Hala M. Abo-Dief

Abstract:

Silver nanoparticles (AgNPs) are the subject of important recent interest, present in a large range of applications such as electronics, catalysis, chemistry, energy, and medicine. Metallic nanoparticles are traditionally synthesized by wet chemical techniques, where the chemicals used are quite often toxic and flammable. In this work, we describe an effective and environmental-friendly technique of green synthesis of silver nanoparticles. Silver nanoparticles (AgNPs) synthesized using silver nitrate solution and the extract of mint, basil, orange peel and Tangerines peel which used as reducing agents. Silver Nanoparticles were characterized using Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and UV–Vis absorption spectroscopy. SEM analysis showed the average particle size of mint, basil, orange peel, Tangerines peel are 30, 20, 12, 10 nm respectively. This is for the first time that any plant extract was used for the synthesis of nanoparticles.

Keywords: silver nanoparticles, green synthesis, scanning electron microscopy, plants

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Authors: Maryam Kiani

Abstract:

This study focuses on the development of composite nanomaterials based on SiO₂ and carbon black for oxygen reduction reaction (ORR) electrocatalysts in batteries and fuel cells. The aim was to explore the potential of these composite materials as efficient catalysts for ORR, which is a critical process in energy conversion devices. The SiO₂/carbon black composite nanomaterials were synthesized using a facile and scalable method. The morphology, structure, and electrochemical properties of the materials were characterized using various techniques including scanning electron microscopy (SEM), X-ray diffraction (XRD), and electrochemical measurements. The results demonstrated that the incorporation of SiO₂ into the carbon black matrix enhanced the ORR performance of the composite material. The composite nanomaterials exhibited improved electrocatalytic activity, enhanced stability, and increased durability compared to pure carbon black. The presence of SiO₂ facilitated the formation of active sites, improved electron transfer, and increased the surface area available for ORR. This study contributes to the advancement of battery and fuel cell technology by offering a promising approach for the development of high-performance ORR electrocatalysts. The SiO₂/carbon black composite nanomaterials show great potential for improving the efficiency and durability of energy conversion devices, leading to more sustainable and efficient energy solutions.

Keywords: ORR, fuel cells, batteries, electrocatalyst

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