Search results for: Electrochemical analysis

Authors: Christian C. Vaso, Rinlee Butch M. Cervera

Abstract:

One of the most promising anode materials for solid oxide electrolysis cell (SOEC) application is the Sr-doped LaMnO₃ (LSM) which is known to have a high electronic conductivity but low ionic conductivity. To increase the ionic conductivity or diffusion of ions through the anode, Yttria-stabilized Zirconia (YSZ), which has good ionic conductivity, is proposed to be combined with LSM to create a composite electrode and to obtain a high mixed ionic and electronic conducting anode. In this study, composite of lanthanum strontium manganite and YSZ oxide, La_0.8Sr_0.2MnO₃/Zr_0.92Y_0.08O₂ (LSM/YSZ), with different wt.% compositions of LSM and YSZ were synthesized using solid-state reaction. The obtained prepared composite samples of 60, 50, and 40 wt.% LSM with remaining wt.% of 40, 50, and 60, respectively for YSZ were fully characterized for its microstructure by using powder X-ray diffraction (XRD), Thermogravimetric analysis (TGA), Fourier transform infrared (FTIR), and Scanning electron microscope/Energy dispersive spectroscopy (SEM/EDS) analyses. Surface morphology of the samples via SEM analysis revealed a well-sintered and densified pure LSM, while a more porous composite sample of LSM/YSZ was obtained. Electrochemical impedance measurements at intermediate temperature range (500-700 °C) of the synthesized samples were also performed which revealed that the 50 wt.% LSM with 50 wt.% YSZ (L50Y50) sample showed the highest total conductivity of 8.27x10^-1 S/cm at 600 ^oC with 0.22 eV activation energy.

Keywords: Ceramics, microstructure, fuel cells, electrochemical impedance spectroscopy.

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Authors: Aniela Pop, Ianina Birsan, Corina Orha, Rodica Pode, Florica Manea

Abstract:

Carbon nanofiber-epoxy composite electrode has been investigated through voltammetric and amperometric techniques in order to detect parabens from aqueous solutions. The occurrence into environment as emerging pollutants of these preservative compounds has been extensively studied in the last decades, and consequently, a rapid and reliable method for their quantitative quantification is required. In this study, methylparaben (MP) and propylparaben (PP) were chosen as representatives for paraben class. The individual electrochemical detection of each paraben has been successfully performed. Their electrochemical oxidation occurred at the same potential value. Their simultaneous quantification should be assessed electrochemically only as general index of paraben class as a cumulative signal corresponding to both MP and PP from solution. The influence of pH on the electrochemical signal was studied. pH ranged between 1.3 and 9.0 allowed shifting the detection potential value to smaller value, which is very desired for the electroanalysis. Also, the signal is better-defined and higher sensitivity is achieved. Differential-pulsed voltammetry and square-wave voltammetry were exploited under the optimum pH conditions to improve the electroanalytical performance for the paraben detection. Also, the operation conditions were selected, i.e., the step potential, modulation amplitude and the frequency. Chronomaprometry application as the easiest electrochemical detection method led to worse sensitivity, probably due to a possible fouling effect of the electrode surface. The best electroanalytical performance was achieved by pulsed voltammetric technique but the selection of the electrochemical technique is related to the concrete practical application. A good reproducibility of the voltammetric-based method using carbon nanofiber-epoxy composite electrode was determined and no interference effect was found for the cation and anion species that are common in the water matrix. Besides these characteristics, the long life-time of the electrode give to carbon nanofiber-epoxy composite electrode a great potential for practical applications.

Keywords: Carbon nanofiber-epoxy composite electrode, electroanalysis, methylparaben, propylparaben.

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Authors: Tze Sian Pui, Tushar Bansal, Patthara Kongsuphol, Sunil K. Arya

Abstract:

We present a label-free biosensor based on electrochemical impedance spectroscopy for the detection of proinflammatory cytokine Tumor Necrosis Factor (TNF-α). Secretion of TNF-α has been correlated to the onset of various diseases including rheumatoid arthritis, Crohn-s disease etc. Gold electrodes were patterned on a silicon substrate and self assembled monolayer of dithiobis-succinimidyl propionate was used to develop the biosensor which achieved a detection limit of ~57fM. A linear relationship was also observed between increasing TNF-α concentrations and chargetransfer resistance within a dynamic range of 1pg/ml – 1ng/ml.

Keywords: Tumor necrosis factor, electrochemical impedance spectroscopy, label free, self assembled monolayer

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Authors: B. D. Polat, O. Keles

Abstract:

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 is 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 nanostructured 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: O. Tovide, N. Jahed, N. Mohammed, C. E. Sunday, H. R. Makelane, R. F. Ajayi, K. M. Molapo, A. Tsegaye, M. Masikini, S. Mailu, A. Baleg, T. Waryo, P. G. Baker, E. I. Iwuoha

Abstract:

A graphenated–polyaniline (GR-PANI) nanocomposite sensor was constructed and used for the determination of anthracene. The direct electro-oxidation behavior of anthracene on the GR-PANI modified glassy carbon electrode (GCE) was used as the sensing principle. The results indicate thatthe response profile of the oxidation of anthracene on GR-PANI-modified GCE provides for the construction of sensor systems based onamperometric and potentiometric signal transductions. A dynamic linear range of 0.12- 100 µM anthracene and a detection limit of 0.044 µM anthracene were established for the sensor system.

Keywords: Electrochemical sensors, environmental pollutants, graphenated-polymers, polyaromatic hydrocarbon.

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Authors: S. Sieniutycz

Abstract:

This paper unifies power optimization approaches in various energy converters, such as: thermal, solar, chemical, and electrochemical engines, in particular fuel cells. Thermodynamics leads to converter-s efficiency and limiting power. Efficiency equations serve to solve problems of upgrading and downgrading of resources. While optimization of steady systems applies the differential calculus and Lagrange multipliers, dynamic optimization involves variational calculus and dynamic programming. In reacting systems chemical affinity constitutes a prevailing component of an overall efficiency, thus the power is analyzed in terms of an active part of chemical affinity. The main novelty of the present paper in the energy yield context consists in showing that the generalized heat flux Q (involving the traditional heat flux q plus the product of temperature and the sum products of partial entropies and fluxes of species) plays in complex cases (solar, chemical and electrochemical) the same role as the traditional heat q in pure heat engines. The presented methodology is also applied to power limits in fuel cells as to systems which are electrochemical flow engines propelled by chemical reactions. The performance of fuel cells is determined by magnitudes and directions of participating streams and mechanism of electric current generation. Voltage lowering below the reversible voltage is a proper measure of cells imperfection. The voltage losses, called polarization, include the contributions of three main sources: activation, ohmic and concentration. Examples show power maxima in fuel cells and prove the relevance of the extension of the thermal machine theory to chemical and electrochemical systems. The main novelty of the present paper in the FC context consists in introducing an effective or reduced Gibbs free energy change between products p and reactants s which take into account the decrease of voltage and power caused by the incomplete conversion of the overall reaction.

Keywords: Power yield, entropy production, chemical engines, fuel cells, exergy.

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

Abstract:

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, microstructure, electrochemical measurements, energy storage, transmission electron microscope.

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Authors: Sarah Fahad Alajmi, Tamer Ezzat Youssef

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Here, we report a simple method for the direct conversion of 6-Nitro-1H-indole into N-substituted indoles via electrochemical dehydrogenative reaction with halogenated reagents under strongly basic conditions through N–R bond formation. The N-protected indoles have been prepared under moderate and scalable electrolytic conditions. The conduct of the reactions was performed in a simple divided cell under constant current without oxidizing reagents or transition-metal catalysts. The synthesized products have been characterized via UV/Vis spectrophotometry, 1H-NMR, and FTIR spectroscopy. A possible reaction mechanism is discussed based on the N-protective products. This methodology could be applied to the synthesis of various biologically active N-substituted indole derivatives.

Keywords: Green chemistry, 1H-indole, NH-containing heteroaromatic, organic electrosynthesis.

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

Abstract:

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

Keywords: Sensors, endocrine disruptors, nanoparticles, electrochemical, microscopy.

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Authors: Taqi Zahid Butt, Tanveer Ahmad Tabish

Abstract:

Martensitic stainless steels have been extensively used for their good corrosion resistance and better mechanical properties. Heat treatment was suggested as one of the most excellent ways to this regard; hence, it affects the microstructure, mechanical and corrosion properties of the steel. In the current research work the microstructural changes and corrosion behavior in an AISI 420A stainless steel exposed to temperatures in the 980-1035oC range were investigated. The heat treatment is carried out in vacuum furnace within the said temperature range. The quenching of the samples was carried out in oil, brine and water media. The formation and stability of passive film was studied by Open Circuit Potential, Potentiodynamic polarization and Electrochemical Scratch Tests. The Electrochemical Impedance Spectroscopy results simulated with Equivalent Electrical Circuit suggested bilayer structure of outer porous and inner barrier oxide films. The quantitative data showed thick inner barrier oxide film retarded electrochemical reactions. Micrographs of the quenched samples showed sigma and chromium carbide phases which prove the corrosion resistance of steel alloy.

Keywords: Martensitic stainless steel corrosion, microstructure, vacuum furnace.

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Authors: Yongkui Cui, Fengping Wang, Hailai Zhao, Muhammad Zubair Iqbal, Ziya Wang, Yan Li, Pengpeng L. V.

Abstract:

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

Keywords: Hydrothermal process, lithium ion battery, Raman spectroscopy, stannous oxide.

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Authors: Jinliang Yuan, Jong-Sung Yu, Bengt Sundén

Abstract:

A computational fluid dynamics (CFD) model is developed for rechargeable non-aqueous electrolyte lithium-air batteries with a partial opening for oxygen supply to the cathode. Multi-phase transport phenomena occurred in the battery are considered, including dissolved lithium ions and oxygen gas in the liquid electrolyte, solid-phase electron transfer in the porous functional materials and liquid-phase charge transport in the electrolyte. These transport processes are coupled with the electrochemical reactions at the active surfaces, and effects of discharge reaction-generated solid Li2O2 on the transport properties and the electrochemical reaction rate are evaluated and implemented in the model. The predicted results are discussed and analyzed in terms of the spatial and transient distribution of various parameters, such as local oxygen concentration, reaction rate, variable solid Li2O2 volume fraction and porosity, as well as the effective diffusion coefficients. It is found that the effect of the solid Li2O2 product deposited at the solid active surfaces is significant on the transport phenomena and the overall battery performance.

Keywords: Computational Fluid Dynamics (CFD), Modeling, Multi-phase, Transport Phenomena, Lithium-air battery.

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Authors: Lawrence I. Onyeji, Girish M. Kale, M. Bijan Kermani

Abstract:

Corrosion problem which exists in every stage of oil and gas production has been a great challenge to the operators in the industry. The conventional carbon steel with all its inherent advantages has been adjudged susceptible to the aggressive corrosion environment of oilfield. This has aroused increased interest in the use of micro alloyed steels for oil and gas production and transportation. The corrosion behavior of three commercially supplied micro alloyed steels designated as A, B, and C have been investigated with API 5L X65 as reference samples. Electrochemical corrosion tests were conducted in an unbuffered 3.5 wt% NaCl solution saturated with CO₂ at 30 ⁰C for 24 hours. Pre-corrosion analyses revealed that samples A, B and X65 consist of ferrite-pearlite microstructures but with different grain sizes, shapes and distribution whereas sample C has bainitic microstructure with dispersed acicular ferrites. The results of the electrochemical corrosion tests showed that within the experimental conditions, the corrosion rate of the samples can be ranked as CR_(A)< CR_(X65)< CR_(B)< CR_(C). These results are attributed to difference in microstructures of the samples as depicted by ASTM grain size number in accordance with ASTM E112-12 Standard and ferrite-pearlite volume fractions determined by ImageJ Fiji grain size analysis software.

Keywords: Carbon dioxide corrosion, corrosion behavior, micro-alloyed steel, microstructures.

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Authors: Amer Dawoud, Rashid Mia, Arati Biswakarma, Jesy Motchaalangaram, Wujan Miao, Karl Wallace

Abstract:

The development of an embedded miniaturized drone-based system for remote detection of Chemical Warfare Agents (CWAs) is proposed. The paper focuses on the software/hardware system design of the electrochemical Cyclic Voltammetry (CV) and Differential Pulse Voltammetry (DPV) signal processing for future deployment on drones. The paper summarizes the progress made towards hardware and electrochemical signal processing for signature detection of CWA. Also, the miniature potentiostat signal is validated by comparing it with the high-end lab potentiostat signal.

Keywords: Drone-based, remote detection chemical warfare agents, miniaturized, potentiostat.

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Authors: Jayesh P. Ruparelia, Bhavna D. Soni

Abstract:

Electrochemical-oxidation of Reactive Black-5 (RB- 5) was conducted for degradation using DSA type Ti/RuO2-SnO2- Sb2O5 electrode. In the study, for electro-oxidation, electrode was indigenously fabricated in laboratory using titanium as substrate. This substrate was coated using different metal oxides RuO2, Sb2O5 and SnO2 by thermal decomposition method. Laboratory scale batch reactor was used for degradation and decolorization studies at pH 2, 7 and 11. Current density (50mA/cm2) and distance between electrodes (8mm) were kept constant for all experiments. Under identical conditions, removal of color, COD and TOC at initial pH 2 was 99.40%, 55% and 37% respectively for initial concentration of 100 mg/L RB-5. Surface morphology and composition of the fabricated electrode coatings were characterized using scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) respectively. Coating microstructure was analyzed by X-ray diffraction (XRD). Results of this study further revealed that almost 90% of oxidation occurred within 5-10 minutes.

Keywords: Electrochemical-oxidation, RB- dye, Decolorization.

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Authors: Yusmeeraz Yusof, Yoshiyuki Yanagimoto, Shigeyasu Uno, Kazuo Nakazato

Abstract:

We demonstrate a nonfaradaic electrochemical impedance spectroscopy measurement of biochemically modified gold plated electrodes using a two-electrode system. The absence of any redox indicator in the impedance measurements provide more precise and accurate characterization of the measured bioanalyte at molecular resolution. An equivalent electrical circuit of the electrodeelectrolyte interface was deduced from the observed impedance data of saline solution at low and high concentrations. The detection of biomolecular interactions was fundamentally correlated to electrical double-layer variation at modified interface. The investigations were done using 20mer deoxyribonucleic acid (DNA) strands without any label. Surface modification was performed by creating mixed monolayer of the thiol-modified single-stranded DNA and a spacer thiol (mercaptohexanol) by a two-step self-assembly method. The results clearly distinguish between the noncomplementary and complementary hybridization of DNA, at low frequency region below several hundreds Hertz.

Keywords: Biosensor, electrical double-layer, impedance spectroscopy, label free DNA.

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Authors: Jafar Khan Kasi, Ajab Khan Kasi, Muzamil Bokhari

Abstract:

Carbon nanotube is one of the most attractive materials for the potential applications of nanotechnology due to its excellent mechanical, thermal, electrical and optical properties. In this paper we report a supercapacitor made of nickel foil electrodes, coated with multiwall carbon nanotubes (MWCNTs) thin film using electrophoretic deposition (EPD) method. Chemical vapor deposition method was used for the growth of MWCNTs and ethanol was used as a hydrocarbon source. High graphitic multiwall carbon nanotube was found at 750oC analyzing by Raman spectroscopy. We observed the electrochemical performance of supercapacitor by cyclic voltammetry. The electrodes of supercapacitor fabricated from MWCNTs exhibit considerably small equivalent series resistance (ESR), and a high specific power density. Electrophoretic deposition is an easy method in fabricating MWCNT electrodes for high performance supercapacitor.

Keywords: Carbon nanotube, chemical vapor deposition, catalyst, charge, cyclic voltammetry.

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Authors: Ingy N. Bkrey, Ahmed A. Moniem

Abstract:

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

Keywords: Electrode Deposition, Flexible, Graphene oxide, Graphene, High Power CO2 Laser, MnO2.

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Authors: A. Talapatra, N. R. Bandhyopadhyay, J. Datta

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In the present study, two TRIP-assisted steels were designated as A (having no Cr and Cu content) and B (having higher Ni, Cr and Cu content) heat treated under different conditions, and the correlation between its heat treatment, microstructure and properties were investigated. Micro structural examination was carried out by optical microscope and scanning electron microscope after electrolytic etching. Non-destructive electrochemical and ultrasonic testing on two TRIP-assisted steels was used to find out corrosion and mechanical properties of different alter microstructure phase’s steels. Furthermore, micro structural studies accompanied by the evaluation of mechanical properties revealed that steels having martensite phases with higher corrosive and hardness value were less sound velocity and also steel’s microstructure having finer grains that was more grain boundary was less corrosion resistance. Steel containing more Cu, Ni and Cr was less corrosive compared to other steels having same processing or microstructure.

Keywords: TRIP-assisted steels, heat treatment, corrosion, electrochemical techniques, micro-structural characterization, non-destructive (ultrasonic) technique.

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Authors: S. Tunmee, P. Wongpanya, I. Toda, X. L. Zhou, Y. Nakaya, N. Konkhunthot, S. Arakawa, H. Saitoh

Abstract:

The hydrogenated amorphous carbon films (α-C:H) were deposited on p-type Si (100) substrates at different thicknesses by radio frequency plasma enhanced chemical vapor deposition technique (rf-PECVD). Raman spectra display asymmetric diamond-like carbon (DLC) peaks, representative of the α-C:H films. The decrease of intensity ID/IG ratios revealed the sp3 content arise at different thicknesses of the α-C:H films. In terms of mechanical properties, the high hardness and elastic modulus values showed the elastic and plastic deformation behaviors related to sp3 content in amorphous carbon films. Electrochemical properties showed that the α-C:H films exhibited excellent corrosion resistance in air-saturated 3.5 wt.% NaCl solution for pH 2 at room temperature. Thickness increasing affected the small sp2 clusters in matrix, restricting the velocity transfer and exchange of electrons. The deposited α-C:H films exhibited excellent mechanical properties and corrosion resistance.

Keywords: Thickness, Mechanical properties, Electrochemical corrosion properties, α-C:H film.

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Authors: Khaled Alawadhi, Abdulkareem Aloraier, Suraj Joshi, Jalal Alsarraf

Abstract:

The aim of this paper is to compare the effectiveness and electrochemical behavior of typical oilfield corrosion inhibitors with previous oilfield corrosion inhibitors under the same electrochemical techniques to control preferential weld corrosion of X65 pipeline steel in artificial seawater saturated with carbon dioxide at a pressure of one bar. A secondary aim is to investigate the conditions under which current reversal takes place. A flow channel apparatus was used in the laboratory to simulate the actual condition that occurs in marine pipelines. Different samples from the parent metal, the weld metal and the heat affected zone in the pipeline steel were galvanically coupled. The galvanic currents flowing between the weld regions were recorded using zero-resistance ammeters and tested under static and flowing conditions in both inhibited and uninhibited media. The results show that a current reversal took place when 30ppm of both green oilfield inhibitors were present, resulting in accelerated weld corrosion.

Keywords: Carbon dioxide, carbon steel, current reversal, inhibitor, weld corrosion.

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Authors: Ayo S. Afolabi, Johannes H. Potgieter, Ambali S. Abdulkareem, Nonhlanhla Fungura

Abstract:

The effect of different tempering temperatures and heat treatment times on the corrosion resistance of austenitic stainless steels in oxalic acid was studied in this work using conventional weight loss and electrochemical measurements. Typical 304 and 316 stainless steel samples were tempered at 150oC, 250oC and 350oC after being austenized at 1050oC for 10 minutes. These samples were then immersed in 1.0M oxalic acid and their weight losses were measured at every five days for 30 days. The results show that corrosion of both types of ASS samples increased with an increase in tempering temperature and time and this was due to the precipitation of chromium carbides at the grain boundaries of these metals. Electrochemical results also confirm that the 304 ASS is more susceptible to corrosion than 316 ASS in this medium. This is attributed to the molybdenum in the composition of the latter. The metallographic images of these samples showed non–uniform distribution of precipitated chromium carbides at the grain boundaries of these metals and unevenly distributed carbides and retained austenite phases which cause galvanic effects in the medium.

Keywords: ASS, corrosion, oxalic acid, tempering, temperature, time.

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Authors: M. Ardelean, F. Manea, A. Pop, J. Schoonman

Abstract:

The presence of pharmaceuticals in the environment and especially in water has gained increasing attention. They are included in emerging class of pollutants, and for most of them, legal limits have not been set-up due to their impact on human health and ecosystem was not determined and/or there is not the advanced analytical method for their quantification. In this context, the development of various advanced analytical methods for the quantification of pharmaceuticals in water is required. The electrochemical methods are known to exhibit the great potential for high-performance analytical methods but their performance is in direct relation to the electrode material and the operating techniques. In this study, two types of carbon-based electrodes materials, i.e., boron-doped diamond (BDD) and carbon nanofiber (CNF)-epoxy composite electrodes have been investigated through voltammetric techniques for the detection of naproxen in water. The comparative electrochemical behavior of naproxen (NPX) on both BDD and CNF electrodes was studied by cyclic voltammetry, and the well-defined peak corresponding to NPX oxidation was found for each electrode. NPX oxidation occurred on BDD electrode at the potential value of about +1.4 V/SCE (saturated calomel electrode) and at about +1.2 V/SCE for CNF electrode. The sensitivities for NPX detection were similar for both carbon-based electrode and thus, CNF electrode exhibited superiority in relation to the detection potential. Differential-pulsed voltammetry (DPV) and square-wave voltammetry (SWV) techniques were exploited to improve the electroanalytical performance for the NPX detection, and the best results related to the sensitivity of 9.959 µA·µM^-1 were achieved using DPV. In addition, the simultaneous detection of NPX and fluoxetine -a very common antidepressive drug, also present in water, was studied using CNF electrode and very good results were obtained. The detection potential values that allowed a good separation of the detection signals together with the good sensitivities were appropriate for the simultaneous detection of both tested pharmaceuticals. These results reclaim CNF electrode as a valuable tool for the individual/simultaneous detection of pharmaceuticals in water.

Keywords: Boron-doped diamond electrode, carbon nanofiber-epoxy composite electrode, emerging pollutants, pharmaceuticals.

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Authors: C. Photiphitak, P. Rakkwamsuk, P. Muthitamongkol, C. Thanachayanont

Abstract:

TiO2/MgO composite films were prepared by coating the magnesium acetate solution in the pores of mesoporous TiO2 films using a dip coating method. Concentrations of magnesium acetate solution were varied in a range of 1x10-4 – 1x10-1 M. The TiO2/MgO composite films were characterized by scanning electron microscopy (SEM), transmission electron microscropy (TEM), electrochemical impedance spectroscopy(EIS) , transient voltage decay and I-V test. The TiO2 films and TiO2/MgO composite films were immersed in a 0.3 mM N719 dye solution. The Dye-sensitized solar cells with the TiO2/MgO/N719 structure showed an optimal concentration of magnesium acetate solution of 1x10-3 M resulting in the MgO film estimated thickness of 0.0963 nm and giving the maximum efficiency of 4.85%. The improved efficiency of dyesensitized solar cell was due to the magnesium oxide film as the wide band gap coating decays the electron back transfer to the triiodide electrolyte and reduce charge recombination.

Keywords: Magnesium oxide thin film, TiO2/MgO composite films, Electrochemical Impedance Spectrum, Transient voltage decay

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Authors: Anjan Sil, Rajni Sharma, Subrata Ray

Abstract:

The effect of carbon nanofibers (CNFs) on the electrical properties of Poly(vinylidene fluoride-hexafluoropropylene) (P(VdF-HFP)) based gel polymer electrolytes has been investigated in the present work. The length and diameter ranges of CNFs used in the present work are 5-50 μm and 200-600 nm respectively. The nanocomposite gel polymer electrolytes have been synthesized by solution casting technique with varying CNFs content in terms of weight percentage. Electrochemical impedance analysis demonstrates that the reinforcement of carbon nanofibers significantly enhances the ionic conductivity of the polymer electrolyte. The decrease of crystallinity of P(VdF-HFP) due the addition of CNFs has been confirmed by X-ray diffraction (XRD). The interaction of CNFs with various constituents of nanocomposite gel polymer electrolytes has been assessed by Fourier Transform Infrared (FTIR) spectroscopy. Moreover CNFs added gel polymer electrolytes offer superior thermal stability as compared to that of CNFs free electrolytes as confirmed by Thermogravimetric analysis (TGA).

Keywords: Polymer electrolytes, CNFs, Ionic conductivity, TGA.

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Authors: Marita Pigłowska, Beata Kurc, Maciej Galiński

Abstract:

The application of carbon materials in the branches of the electrochemical industry shows an increasing tendency each year due to the many interesting properties they possess. These are, among others, a well-developed specific surface, porosity, high sorption capacity, good adsorption properties, low bulk density, electrical conductivity and chemical resistance. All these properties allow for their effective use, among others in supercapacitors, which can store electric charges of the order of 100 F due to carbon electrodes constituting the capacitor plates. Coals (including expanded graphite, carbon black, graphite carbon fibers, activated carbon) are commonly used in electrochemical methods of removing oil derivatives from water after tanker disasters, e.g., phenols and their derivatives by their electrochemical anodic oxidation. Phenol can occupy practically the entire surface of carbon material and leave the water clean of hydrophobic impurities. Regeneration of such electrodes is also not complicated, it is carried out by electrochemical methods consisting in unblocking the pores and reducing resistances, and thus their reactivation for subsequent adsorption processes. Graphite is commonly used as an anode material in lithium-ion cells, while due to the limited capacity it offers (372 mAh g-1), new solutions are sought that meet both capacitive, efficiency and economic criteria. Increasingly, biodegradable materials, green materials, biomass, waste (including agricultural waste) are used in order to reuse them and reduce greenhouse effects and, above all, to meet the biodegradability criterion necessary for the production of lithium-ion cells as chemical power sources. The most common of these materials are cellulose, starch, wheat, rice, and corn waste, e.g., from agricultural, paper and pharmaceutical production. Such products are subjected to appropriate treatments depending on the desired application (including chemical, thermal, electrochemical). Starch is a biodegradable polysaccharide that consists of polymeric units such as amylose and amylopectin that build an ordered (linear) and amorphous (branched) structure of the polymer. Carbon is also used as a catalyst. Elemental carbon has become available in many nano-structured forms representing the hybridization combinations found in the primary carbon allotropes, and the materials can be enriched with a large number of surface functional groups. There are many examples of catalytic applications of coal in the literature, but the development of this field has been hampered by the lack of a conceptual approach combining structure and function and a lack of understanding of material synthesis. In the context of catalytic applications, the integrity of carbon environmental management properties and parameters such as metal conductivity range and bond sequence management should be characterized. Such data, along with surface and textured information, can form the basis for the provision of network support services.

Keywords: carbon materials, catalysis, BET, capacitors, lithium ion cell

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Authors: Julieta D. Chelaru, Maria Gorea

Abstract:

The massive demolition of old buildings in recent years has generated tons of waste, especially brick waste. Thus, a concern of recent research is the use of this waste for the production of environmentally friendly concrete. At the same time, corrosion of the reinforcement steel rebar in classical concrete is a current problem. In this context, in the present paper a study was carried out on the corrosion of metal reinforcement in cement mortars with added brick waste. The corrosion process was analyzed on four compositions of mortars without and with 15%, 25% and 35% brick waste replacing the sand. The brick waste has majority content in SiO2, Al2O3, FeO3 and CaO. The grain size distribution of brick waste was close to that of the sand (dmax = 2 mm). The preparation method of the samples was similar to ordinary mortars. The corrosion action on the rebar in concrete, at different brick waste concentrations, was investigated by electrochemical measurements (polarization curves and electrochemical impedance spectroscopy (EIS)) at 1 month and 26 months. The results obtained at 26 months revealed that the addition of the brick waste in mortar improved the anticorrosion properties in the case of all samples compared with the etalon mortar. The best results were obtained in the case of the sample with 15% brick waste (the efficiency was ≈ 90%). The corrosion intermediary layer formed on the rebar surface was evidenced by SEM-EDX.

Keywords: EIS, steel corrosion, steel reinforced concrete, waste materials.

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Authors: Mandlenkosi George Robert Mahlobo, Peter Apata Olubambi, Philippe Refait

Abstract:

The aim of this study was to use voltammetry as a method to understand the behavior of steel in unsaturated soil in the presence of cathodic protection (CP). Three carbon steel coupons were buried in artificial soil wetted at 65-70% of saturation for 37 days. All three coupons were left at open circuit potential (OCP) for the first seven days in the unsaturated soil before CP which was only applied on two of the three coupons at the protection potential -0.8 V vs. Cu/CuSO4 for the remaining 30 days of the experiment. Voltammetry was performed weekly on the coupon without CP while electrochemical impedance spectroscopy (EIS) was performed daily to monitor and correct the applied CP potential from ohmic drop. Voltammetry was finally performed the last day on the coupons under CP. All the voltammograms were modeled with mathematical equations in order to compute the electrochemical parameters and subsequently deduce the corrosion rate of the steel coupons. For the coupon without CP, the corrosion rate was determined at 300 µm/y. For the coupons under CP, the residual corrosion rate under CP was estimated at 12 µm/y while the corrosion rate of the coupons, after interruption of CP, was estimated at 25 µm/y. This showed that CP was efficient due to two effects: a direct effect, from the decreased potential, and an induced effect, associated with the increased interfacial pH that promoted the formation of a protective layer on the steel surface.

Keywords: Carbon steel, cathodic protection, voltammetry, unsaturated soil, Raman spectroscopy.

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Authors: Anuruddha Jayasuriya, Thanakorn Pheeraphan

Abstract:

In this paper, a review of different mathematical models which can be used as prediction tools to assess the time to crack reinforced concrete (RC) due to corrosion is investigated. This investigation leads to an experimental study to validate a selected prediction model. Most of these mathematical models depend upon the mechanical behaviors, chemical behaviors, electrochemical behaviors or geometric aspects of the RC members during a corrosion process. The experimental program is designed to verify the accuracy of a well-selected mathematical model from a rigorous literature study. Fundamentally, the experimental program exemplifies both one-dimensional chloride diffusion using RC squared slab elements of 500 mm by 500 mm and two-dimensional chloride diffusion using RC squared column elements of 225 mm by 225 mm by 500 mm. Each set consists of three water-to-cement ratios (w/c); 0.4, 0.5, 0.6 and two cover depths; 25 mm and 50 mm. 12 mm bars are used for column elements and 16 mm bars are used for slab elements. All the samples are subjected to accelerated chloride corrosion in a chloride bath of 5% (w/w) sodium chloride (NaCl) solution. Based on a pre-screening of different models, it is clear that the well-selected mathematical model had included mechanical properties, chemical and electrochemical properties, nature of corrosion whether it is accelerated or natural, and the amount of porous area that rust products can accommodate before exerting expansive pressure on the surrounding concrete. The experimental results have shown that the selected model for both one-dimensional and two-dimensional chloride diffusion had ±20% and ±10% respective accuracies compared to the experimental output. The half-cell potential readings are also used to see the corrosion probability, and experimental results have shown that the mass loss is proportional to the negative half-cell potential readings that are obtained. Additionally, a statistical analysis is carried out in order to determine the most influential factor that affects the time to corrode the reinforcement in the concrete due to chloride diffusion. The factors considered for this analysis are w/c, bar diameter, and cover depth. The analysis is accomplished by using Minitab statistical software, and it showed that cover depth is the significant effect on the time to crack the concrete from chloride induced corrosion than other factors considered. Thus, the time predictions can be illustrated through the selected mathematical model as it covers a wide range of factors affecting the corrosion process, and it can be used to predetermine the durability concern of RC structures that are vulnerable to chloride exposure. And eventually, it is further concluded that cover thickness plays a vital role in durability in terms of chloride diffusion.

Keywords: Accelerated corrosion, chloride diffusion, corrosion cracks, passivation layer, reinforcement corrosion.

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Authors: W. Walke, J. Przondziono, K. Nowińska

Abstract:

The study comprises evaluation of suitability of passive layer created on the surface of AISI 316L stainless steel for products that are intended to have contact with blood. For that purpose, prior to and after chemical passivation, samples were subject to 7 day exposure in artificial plasma at the temperature of T=37°C. Next, tests of metallic ions infiltration from the surface to the solution were performed. The tests were performed with application of spectrometer JY 2000, by Yobin – Yvon, employing Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). In order to characterize physical and chemical features of electrochemical processes taking place during exposure of samples to artificial plasma, tests with application of electrochemical impedance spectroscopy were suggested. The tests were performed with application of measuring unit equipped with potentiostat PGSTAT 302n with an attachment for impedance tests FRA2. Measurements were made in the environment simulating human blood at the temperature of T=37°C. Performed tests proved that application of chemical passivation process for AISI 316L stainless steel used for production of goods intended to have contact with blood is well-grounded and useful in order to improve safety of their usage.

Keywords: AISI 316L stainless steel, chemical passivation, artificial plasma, ions infiltration, EIS.

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