• Title/Summary/Keyword: Scanning Electrochemical Microscopy

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Experimental and Theoretical Studies on Corrosion Inhibition Performance of Phenanthroline for Cast Iron in Acid Solution

  • Idir, B.;Kellou-Kerkouche, F.
    • Journal of Electrochemical Science and Technology
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    • v.9 no.4
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    • pp.260-275
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    • 2018
  • The corrosion inhibition of cast iron in 1 M HCl by Phenanthroline (Phen) was investigated using potentiodynamic polarization (PDP) curves, electrochemical impedance spectroscopy (EIS), surface analysis and theoretical calculations. It is found that Phen exhibits high inhibition activity towards the corrosive action of HCl and its adsorption obeys the Langmuir adsorption isotherm model. The results showed that inhibition efficiency increases with Phen concentration up to a maximum value of 96% at 1.4 mM, and decreases slightly with the increase in temperature. The free adsorption energy value indicates that Phen adsorbs on cast iron surface in 1 M HCl via a simultaneous physisorption and chemisorption mechanism. Scanning electron microscopy (SEM) micrographs, atomic force microscopy (AFM) and FTIR analysis confirmed the formation of a protective film on cast iron surface, resulting in the improvement of its corrosion resistance in the studied aggressive solution. Quantum chemical calculations at the DFT level were achieved to correlate electronic structure parameters of Phen molecules with their adsorption mode.

Corrosion behaviors of plasma electrolytic oxidation (PEO) treated high-silicon aluminum alloys

  • Park, Deok-Yong;Chang, Chong-Hyun;Oh, Yong-Jun;Myung, Nosang V.;Yoo, Bongyoung
    • Journal of the Korean institute of surface engineering
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    • v.55 no.3
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    • pp.143-155
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    • 2022
  • Ceramic oxide layers successfully were formed on the surface of cast Al alloys with high Si contents using plasma electrolytic oxidation (PEO) process in electrolytes containing Na2SiO3, NaOH, and additives. The microstructure of the oxide layers was systematically analyzed using scanning electron microscopy (SEM), cross-sectional transmission electron microscopy (TEM), X-ray diffraction patterns (XRD), and energy X-ray dispersive spectroscopy (EDS). XRD analysis indicated that the PEO untreated high-silicon Al alloys (i.e., 17.1 and 11.7 wt.% Si) consist of Al, Si and Al2Cu phases whereas Al2Cu phase selectively disappeared after PEO treatment. PEO process yielded an amorphous oxide layer with few second phases including γ-Al2O3 and Fe-rich phases. The corrosion behaviors of high-silicon Al alloys treated by PEO process were investigated using electrochemical impedance spectroscopy (EIS) and other electrochemical techniques (i.e., open circuit potential and polarization curve). Electroanalytical studies indicated that high-silicon Al alloys treated by PEO process have greater corrosion resistance than high-silicon alloys untreated by PEO process.

A New Way to Prepare MoO3/C as Anode of Lithium ion Battery for Enhancing the Electrochemical Performance at Room Temperature

  • Yu, Zhian;Jiang, Hongying;Gu, Dawei;Li, Jishu;Wang, Lei;Shen, Linjiang
    • Journal of Electrochemical Science and Technology
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    • v.7 no.2
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    • pp.170-178
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    • 2016
  • Composited molybdenum oxide and amorphous carbon (MoO3/C) as anode material for lithium ion batteries has been successfully synthesized by calcining polyaniline (PANI) doped with ammonium heptamolybdate tetrahydrate (AMo). The as prepared electrode material was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and field emission scanning electron microscopy (FE-SEM). The electrochemical performance of the anode was investigated by galvanostatic charge/discharge, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The MoO3/C shows higher specific capacity, better cyclic performance and rate performance than pristine MoO3 at room temperature. The electrochemical of MoO3/C properties at various temperatures were also investigated. At elevated temperature, MoO3/C exhibited higher specific capacity but suffered rapidly declines. While at low temperature, the electrochemical performance was mainly limited by the low kinetics of lithium ion diffusion and the high charge transfer resistance.

Synthesis, morphology and electrochemical applications of iron oxide based nanocomposites

  • Letti, Camila J.;Costa, Karla A.G.;Gross, Marcos A.;Paterno, Leonardo G.;Pereira-da-Silva, Marcelo A.;Morais, Paulo C.;Soler, Maria A.G.
    • Advances in nano research
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    • v.5 no.3
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    • pp.215-230
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    • 2017
  • The development of hybrid systems comprising nanoparticles and polymers is an opening pathway for engineering nanocomposites exhibiting outstanding mechanical, optical, electrical, and magnetic properties. Among inorganic counterpart, iron oxide nanoparticles (IONP) exhibit high magnetization, controllable surface chemistry, spintronic properties, and biological compatibility. These characteristics enable them as a platform for biomedical applications and building blocks for bottom-up approaches, such as the layer-by-layer (LbL). In this regard, the present study is addressed to investigate IONP synthesised through co-precipitation route (average diameter around 7 nm), with either positive or negative surface charges, LbL assembled with sodium sulfonated polystyrene (PSS) or polyaniline (PANI). The surface and internal morphologies, and electrochemical properties of these nanocomposites were probed with atomic force microscopy, UV-vis and Raman spectroscopy, scanning electron microscopy, cross-sectional transmission electron microscopy, and electrochemical measurements. The nanocomposites display a globular morphology with IONP densely packed while surface dressed by polyelectrolytes. The investigation of the effect of thermal annealing (300 up to $600^{\circ}C$) on the oxidation process of IONP assembled with PSS was performed using Raman spectroscopy. Our findings showed that PSS protects IONP from oxidation/phase transformation to hematite up to $400^{\circ}C$. The electrochemical performance of nanocomposite comprising IONP and PANI were investigated in $0.5mol{\times}L^{-1}$ $Na_2SO_4$ electrolyte solution by cyclic voltammetry and chronopotentiometry. Our findings indicate this structure as promising candidate for potential application as electrodes for supercapacitors.

The Ways for Bi on Pt to Enhance Formic Acid Oxidation

  • Hyein Lee;Young Jun Kim;Youngku Sohn;Choong Kyun Rhee
    • Journal of Electrochemical Science and Technology
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    • v.14 no.1
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    • pp.21-30
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    • 2023
  • This work presents a correlation between the behavior of formic acid oxidation (FAO) on various Bi-modified Pt(poly) disk electrodes and their morphologies observed on Bi-modified Pt(111) disk electrodes using electrochemical scanning tunneling microscopy (EC-STM) to understand the effects of Bi on Pt. To distinguish the FAO activities of Bi on Pt and plain Pt around Bi, additional Pt was intentionally deposited using two different routes: direct route and iodine route. In direct route, Pt was directly deposited on Bi islands and plain Pt sites around Bi islands, while in iodine route, Pt was exclusively deposited on Bi islands by protecting plain Pt sites with adsorbed iodine. Thus, a comparison of FAO performances on the two Bi-modified Pt electrodes with additional Pt (deposited in the different ways) disclosed a difference in FAO performances on plain Pt sites and Bi islands. When Bi coverage was ~0.04, the Bi deposits were scattered Bi islands enhancing FAO on Pt(poly). The additional Pt deposits using direct route increased FAO efficiency, while the ones using iodine route slightly decreased FAO current. The EC-STM observations indicated that Pt deposits around Bi islands, not on Bi islands, were responsible for the FAO current increase on Bi-modified Pt(poly). The FAO efficiency on Bi-modified Pt(poly) with a Bi coverage of ~0.25 increased by a factor of 2. However, the additional Pt deposits using the two Pt deposition routes notably decreased the FAO current. The dependency of FAO on Bi coverage was discussed in terms of electronic effect and ensemble effect.

Fabrication and Characterization of Pyrolyzed Carbon for Use as an Electrode Material in Electrochemical Biosensor (전기화학 바이오센서의 전극물질로 응용을 위한 열분해 탄소의 제작 및 특성 연구)

  • Lee, Jung-A.;Hwang, Seong-Pil;Kwak, Ju-Hyoun;Park, Se-Il;Lee, Seung-Seob;Lee, Kwang-Cheol
    • Transactions of the Korean Society of Mechanical Engineers A
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    • v.31 no.10
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    • pp.986-992
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    • 2007
  • This paper presents the fabrication and characterization of carbon films pyrolyzed with various photoresists for bioMEMS applications. To verify the usefulness of pyrolyzed carbon films as an electrode material in an electrochemical biosensor developed by the authors, interactions between avidin and biotin on the pyrolyzed carbon film were studied via electrochemical impedance spectroscopy based on electrostatic interactions between avidin and negatively-charged ferricyanide. The pyrolyzed carbon films were characterized using a surface profiler, a precision semiconductor parameter analyzer, a nanoindentor, scanning electron microscopy, and atomic force microscopy. Amine conjugated biotin was immobilized on the electrode using EDC/NHS as crosslinkers after $O_2$ plasma treatment to enhance functional groups on the carbon electrode pyrolyzed at $1000^{\circ}C$ with AZ9260. The detection of avidin binding with different concentrations in a range of 0.75 nM to $7.5\;{\mu}M$ to the pyrolyzed carbon electrode modified with biotin was carried out by measuring the electrochemical impedance change. The results show that avidin binds to the biotin on the electrode not by non-specific interaction but by specific interaction, and that EIS successfully detects this binding event. Pyrolyzed carbon films are a promising material for miniaturization, integration, and low-cost fabrication in electrochemical biosensors.

Modified Glassy Carbon Electrode with Silver Nanoparticles/Polyaniline/Reduced Graphene Oxide Nanocomposite for the Simultaneous Determination of Biocompounds in Biological Fluids

  • Ghanbari, Kh.;Moloudi, M.;Bonyadi, S.
    • Journal of Electrochemical Science and Technology
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    • v.10 no.4
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    • pp.361-372
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    • 2019
  • The silver nanoparticles/polyaniline/reduced graphene oxide nanocomposite modified glassy carbon electrode (Ag/PANI/RGO/GCE) was prepared by the electrochemical method. The Ag/PANI/RGO nanocomposite was characterized by transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), Raman spectroscopy, X-ray diffraction (XRD), and electrochemical impedance spectroscopy (ESI). Two electrochemical techniques namely differential pulse voltammetry (DPV) and cyclic voltammetry (CV) were used to the electrochemical behaviors investigation of ascorbic acid (AA), dopamine (DA), and uric acid (UA). The Ag/PANI/RGO/GCE exhibited remarkable electrocatalytic activity towards the oxidation reaction of AA, DA, and UA in Britton-Robinson (BR) solution (pH=4.0). Under the optimal conditions, the determinations of AA, DA, and UA were accomplished using DPV. AA-DA and DA-UA peak potential separations were 130 and 180 mV, respectively. For simultaneous detection, the linear response ranges were in the two concentration ranges of 0.05-0.8 mM and 2.0-16.0 mM with detection limit 0.412 μM (S/N = 3) for AA, 0.7-90.0 μM and 90.0-1000.0 μM with detection limit 0.023 μM (S/N = 3) for DA, and 0.8-70.0 μM and 70.0-1000.0 μM with detection limit 0.050 μM (S/N = 3) for UA. This modified electrode showed good sensitivity, selectivity, and stability with applied to determine AA, DA, and UA in human urine and drug.

Preparation and Electrochemical Properties of LiFePO4-PSS Composite Cathode for Lithium-ion Batteries

  • Nguyen, Hiep Van;Jin, En Mei;Gu, Hal-Bon
    • Transactions on Electrical and Electronic Materials
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    • v.13 no.4
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    • pp.177-180
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    • 2012
  • In this study, we prepared $LiFePO_4$- poly (sodium 4-styrenesulfonate) (PSS) composite by the hydrothermal method and ball-milling process. Different wt% PSS were added to $LiFePO_4$. The cathode electrodes were made from mixtures of $LiFePO_4$-PSS: SP-270: PVDF in a weighting ratio of 70%: 25%: 5%. $LiFePO_4$-PSS powders were characterized by X-ray diffraction (XRD), and scanning electron microscopy (SEM). The electrochemical properties of $LiFePO_4$-PSS/Li batteries were analyzed by cyclic voltammetry, charge/discharge tests, and AC impedance spectroscopy. A Li/$LiFePO_4$-PSS battery with 4.75 wt% PSS shows the best electrochemical properties, with a discharge capacity of 128 mAh/g.

Electrochemical characterization of supercapacitors based on carbons derived from Sorona activated by ZnCl2

  • Jisha, M.R.;Christy, Maria;Kim, Ae Rhan;Nahm, Kee Suk;Yoo, Dong Jin
    • Journal of Energy Engineering
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    • v.21 no.3
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    • pp.309-314
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    • 2012
  • Carbons derived by the pyrolysis of Sorona activated by $ZnCl_2$ in the ratio of 1:20 and non-porogen Sorona carbons are used as the electrode materials in asymmetric electrochemical supercapacitors and electrochemical behavior is investigated. Scanning electron microscopy (SEM) reveals the porogen free carbons show a flake-like structure and the $ZnCl_2$-treated Sorona carbons have a loose, disjoint structure without any particular shape. Cyclic voltammetric (CV) studies show specific prolate rectangular shape and gives good capacitive properties.

Effect of Microstructure on Corrosion Behavior of TiN Hard Coatings Produced by Two Grid-Attached Magnetron Sputtering

  • Kim, Jung Gu;Hwang, Woon Suk
    • Corrosion Science and Technology
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    • v.5 no.1
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    • pp.15-22
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    • 2006
  • The introduction of two-grid inside a conventional process system produces a reactive coating deposition and increases metal ion ratio in the plasma, resulting in denser and smoother films. The corrosion behaviors of TiN coatings were investigated by electrochemical methods, such as potentiodynamic polarization test and electrochemical impedance spectroscopy (EIS) in deaerated 3.5% NaCl solution. Electrochemical tests were used to evaluate the effect of microstructure on the corrosion behavior of TiN coatings exposed to a corrosive environment. The crystal structure of the coatings was examined by X-ray diffractometry (XRD) and the microstructure of the coatings was investigated by scanning electron microscopy (SEM) and transmission electron spectroscopy (TEM). In the potentiodynamic polarization test and EIS measurement, the corrosion current density of TiN deposited by two grid-attached magnetron sputtering was lower than TiN deposited by conventional magnetron type and also presented higher Rct values during 240 h immersion time. It is attributed to the formation of a dense microstructure, which promotes the compactness of coatings and yields lower porosity.