• Title/Summary/Keyword: Scanning electrochemical microscopy

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Determination of Ascorbic Acid, Acetaminophen, and Caffeine in Urine, Blood Serum by Electrochemical Sensor Based on ZnO-Zn2SnO4-SnO2 Nanocomposite and Graphene

  • Nikpanje, Elham;Bahmaei, Manochehr;Sharif, Amirabdolah Mehrdad
    • Journal of Electrochemical Science and Technology
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    • v.12 no.2
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    • pp.173-187
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    • 2021
  • In the present research, a simple electrochemical sensor based on a carbon paste electrode (CPE) modified with ZnO-Zn2SnO4-SnO2 and graphene (ZnO-Zn2SnO4-SnO2/Gr/CPE) was developed for the direct, simultaneous and individual electrochemical measurement of Acetaminophen (AC), Caffeine (Caf) and Ascorbic acid (AA). The synthesized nano-materials were investigated using scanning electron microscopy, X-ray Diffraction, Fourier-transform infrared spectroscopy, and electrochemical impedance spectroscopy techniques. Cyclic voltammetry and differential pulse voltammetry were applied for electrochemical investigation ZnO-Zn2SnO4-SnO2/Gr/CPE, and the impact of scan rate and the concentration of H+ on the electrode's responses were investigated. The voltammograms showed a linear relationship between the response of the electrode for individual oxidation of AA, AC and, Caf in the range of 0.021-120, 0.018-85.3, and 0.02-97.51 μM with the detection limit of 8.94, 6.66 and 7.09 nM (S/N = 3), respectively. Also, the amperometric technique was applied for the measuring of the target molecules in the range of 0.013-16, 0.008-12 and, 0.01-14 μM for AA, AC and, Caf with the detection limit of 6.28, 3.64 and 3.85 nM, respectively. Besides, the ZnO-Zn2SnO4-SnO2/Gr/CPE shows an excellent selectivity, stability, repeatability, and reproducibility for the determination of AA, AC and, Caf. Finally, the proposed sensor was successfully used to show the amount of AA, AC and, Caf in urine, blood serum samples with recoveries ranging between 95.8% and 104.06%.

Physicochemical and Electrochemical Characteristics of Carbon Nanomaterials and Carbon Nanomaterial-Silicon Composites

  • Kim, Soo-Jin;Hyun, Yura;Lee, Chang-Seop
    • Journal of the Korean Chemical Society
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    • v.60 no.5
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    • pp.299-309
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    • 2016
  • In this study, the physicochemical and electrochemical properties of carbon nanomaterials and synthesized nano-carbon/Si composites were studied. The nano-carbon/Si composites were ball-milled to a nano size and coated with pyrolytic carbon using Chemical Vapor Deposition (CVD). They were then finely mixed with respective nano-carbon materials. The physicochemical properties of samples were analyzed using Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), Raman spectroscopy, X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), and surface area analyzer. The electrochemical characteristics were investigated using the galvanostatic charge-discharge and cyclic voltammetry (CV) measurements. Three-electrode cells were fabricated using the carbon nanomaterials and nano-carbon/Si composites as anode materials and LiPF6 and LiClO4 as electrolytes of Li secondary batteries. Reversibility using LiClO4 as an electrolyte was superior to that of LiPF6 as the electrolyte. The initial discharge capacities of nano-carbon/Si composites were increased compared to the initial discharge capacities of nano-carbon materials.

Electrochemical Performance of Li4Ti5O12 Particles Manufactured Using High Pressure Synthesis Process for Lithium Ion Battery (초고압 합성법으로 제조한 리튬이온전지 음극활물질 Li4Ti5O12의 전기화학적 특성)

  • Ji, Sung Hwa;Jo, Wan Taek;Kim, Hyun Hyo;Kim, Hyojin
    • Korean Journal of Materials Research
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    • v.28 no.6
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    • pp.337-342
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    • 2018
  • Using a high pressure homonizer, we report on the electrochemical performance of $Li_4Ti_5O_{12}(LTO)$ particles manufactured as anode active material for lithium ion battery. High-pressure synthesis processing is performed under conditions in which the mole fraction of Li/Ti is 0.9, the synthesis pressure is 2,000 bar and the numbers of passings-through are 5, 7 and 10. The observed X-ray diffraction patterns show that pure LTO is manufactured when the number of passings-through is 10. It is found from scanning electron microscopy analysis that the average size of synthesized particles decreases as the number of passings-through increases. $LiCoO_2-based$ active cathode materials are used to fabricate several coin half/full cells and their battery characteristics such as lifetime, rate capability and charge transfer resistance are then estimated, revealing quite good electrochemical performance of the LTO particles as an effective anode active material for lithium secondary batteries.

Adsorption properties and metal growth aspects on the surface of activated carbon monolith electrochemically deposited with Ag

  • Oh, Won-Chun;Lim, Chang-Sung
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.14 no.2
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    • pp.37-46
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    • 2004
  • The electrochemical adsorption of the Ag ions from aqueous solution on pelletized activated carbon monolith was investigated over wide range of operation time. The adsorption capacities of pelletized activated carbon monolith are associated with their internal porosity and are related properties such as surface area, pore size distribution. The chemical industry generates wastewater that contains toxic matters like heavy metals in small concentrations so that their economic recovery is not feasible. But, the method using activated carbon monolith can be used to withdrawal of heavy metals in waste water. After the electrochemical treatment, the quantitative properties in Ag ion solutions are also examined by pH concentration and studied elemental analysis by ICP-Atomic Emission Spectrometer and Energy Disperse X-ray (EDX) spectra. It is consider that the pH is very important factor at the reason of water pollutant with increasing acidity in industrial field. The result of quantitative analysis using Inductively Coupled Plasma-Atomic Emission Spectrometer of metal after electrochemical reaction in Ag ions solution depending on time are shown that the amount of Ag ions deposited was decreased with growth of Ag particles on the carbon surfaces as increasing electrochemically treated time. And, surface morphologies are investigated by scanning electron microscopy (SEM) to explain the changes in adsorption properties.

Electrochemical Properties of Carbon Nano-Tube Electrode (탄소나노튜브 전극의 전기화학적 특성)

  • Lee Dong-Yoon;Koo Bo-Kun;Lee Won-Jae;Song Jae-Sung;Kim Hyun-Ju
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.54 no.4
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    • pp.139-143
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    • 2005
  • For application of carbon nano-tube (CNT) as a counter electrode materials of dye-sensitized solar cell (DSSC), the electrochemical behavior of CNT electrode was studied, employing cyclic-voltammetry (C-V) and impedance spectroscopy. Fabrication of CNT-paste and formation of CNT-counter electrode for characteristic measurement have been carried out using ball-milling and doctor blade process, respectively. Unit cell for measurements was assembled using Pt electrode, CNT electrode, and iodine-embedded electrolyte. Field emission-scanning electron microscopy (FE-SEM) was used for structural investigation of CNT powder and electrode. Sheet resistance of electrode was measured with 4-point probe method. Electrochemical properties of electrode, C-V and impedance spectrum, were studied, employing potentiogalvanostat (EG&G 273A) and lock in amplifier (EG&G 5210). As a results, the sheet resistance of CNT electrode is almost similar to that of F-doped SnO2 (FTO) coated glass substrate as approximately 10 ohm/sq. From C-V and impedance spectroscopy measurements, it was found that CNT electrode has high reaction rate and low interface reaction resistance between CNT surface and electrolyte. These results provides that CNT electrode were superior to that of conventional Pt electrode. Particularly, the reaction rate in the CNT electrode is about thrice high than Pt electrode. Therefore. CNT electrode is to be good candidate material for counter electrode in DSSC.

Control of Surface Chemistry and Electrochemical Performance of Carbon-coated Silicon Anode Using Silane-based Self-Assembly for Rechargeable Lithium Batteries

  • Choi, Hyun;Nguyen, Cao Cuong;Song, Seung-Wan
    • Bulletin of the Korean Chemical Society
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    • v.31 no.9
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    • pp.2519-2526
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    • 2010
  • Silane-based self-assembly was employed for the surface modification of carbon-coated Si electrodes and their surface chemistry and electrochemical performance in battery electrolyte depending on the molecular structure of silanes was studied. IR spectroscopic analyses revealed that siloxane formed from silane-based self-assembly possessed Si-O-Si network on the electrode surface and high surface coverage siloxane induced the formation of a stable solid-electrolyte interphase (SEI) layer that was mainly composed of organic compounds with alkyl and carboxylate metal salt functionalities, and PF-containing inorganic species. Scanning electron microscopy imaging showed that particle cracking were effectively reduced on the carbon-coated Si when having high coverage siloxane and thickened SEI layer, delivering > 1480 mAh/g over 200 cycles with enhanced capacity retention 74% of the maximum discharge capacity, in contrast to a rapid capacity fade with low coverage siloxane.

Fluoroethylene Carbonate Addition Effect on Electrochemical Properties of Mixed Carbonate-based Organic Electrolyte Solution for a Capacitor

  • Kim, Mingyeong;Kim, Ick-Jun;Yang, Sunhye;Kim, Seok
    • Bulletin of the Korean Chemical Society
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    • v.35 no.2
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    • pp.466-470
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    • 2014
  • In this paper, organic solvent electrolytes were prepared by a mixture of propylene carbonate (PC), dimethyl carbonate (DMC), tetraethylammonium tetrafluoroborate ($TEABF_4$)s to evaluate the ionic properties of propylene carbonate (PC)/dimethyl carbonate (DMC) mixtures as solvents for a capacitor application, in view of improving the electrochemical performances. The bulk resistance and interfacial resistance of the mixture electrolytes were investigated using an AC impedance method. The morphology of carbon-based electrodes which were contained in different electrolytes was analyzed by scanning electron microscopy (SEM) method. From the experimental results, by increasing the FEC content, capacitance of electrodes was increased, and the interfacial resistance was decreased. In particular, by a content of 2 vol % FEC in 0.2 M $TEABF_4$ PC/DMC solvent, the electrolyte showed the superior capacitance. However, when FEC content exceeds 2 vol %, the capacitance was decreased and the interfacial resistance was increased.

Electrochemical Properties of Li[Ni0.2Li0.2Mn0.6]O2 by Microwave-assisted Sol-gel Method

  • Park, Yong-Joon;Kim, Seuk-Buom
    • Transactions on Electrical and Electronic Materials
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    • v.10 no.3
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    • pp.102-105
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    • 2009
  • $Li[Ni_{0.2}Li_{0.2}Mn_{0.6}]O_2$ cathode materials have been synthesized by a microwave-assisted sol-gel method. The structure and electrochemical properties of $Li[Ni_{0.2}Li_{0.2}Mn_{0.6}]O_2$ were studied by X-ray difftactometry (XRD), scanning electron microscopy (SEM) and charge-discharge cycler. The powder prepared by microwave assisted sol-gel method showed good crystallinity and well-defined facet shapes. The $Li[Ni_{0.2}Li_{0.2}Mn_{0.6}]O_2$ electrode delivered a high discharge capacity of 230 $mAhg^{-1}$ at the specific current of 40 $mAg^{-1}$ (0.2 C rate) in the voltage range of 2.0${\sim}$4.8 V. About 60 % of the discharge capacity measured at 0.2 Crate (140 $mAhg^{-1}$) was maintained at a 6 C (1200 $mAg^{-1}$)rate. The cyclic property was also stable and it did not deteriorated at a high Crate.

Effect of [Al(DMSO2)3]3+ Concentration on Al Electrodeposition from AlCl3/Dimethylsulfone Baths

  • Kim, Sangjae;Matsunaga, Naoya;Kuroda, Kensuke;Okido, Masazumi
    • Journal of Electrochemical Science and Technology
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    • v.9 no.1
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    • pp.69-77
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    • 2018
  • Aluminum electrodeposition was carried out in dimethylsulfone ($DMSO_2$) baths containing 6.2-28.3 mol% $AlCl_3$ at 403 K. The electrochemically active species for Al electrodeposition in $DMSO_2$ baths were investigated. Electrochemical behavior of the electrolyte and the deposition mechanism were studied via cyclic voltammetry (CV). Properties of the deposits were assessed by scanning electron microscopy with energy-dispersive X-ray spectroscopy and X-ray diffraction. In addition, structures of the ionic complexes formed with aluminum in the bath were characterized by $^{27}Al$ nuclear magnetic resonance (NMR) spectroscopy. NMR spectra revealed that all baths contained two ionic species: $AlCl_4{^-}$ and $[Al(DMSO_2)_3]^{3+}$. Al electrodeposited when the $[Al(DMSO_2)_3]^{3+}$ concentration was the highest (23.3 mol% $AlCl_3$) exhibited fine grain sizes, relatively smooth surfaces, and high purities.

Synthesis of CoSe2/RGO Composites and Its Application as a Counter Electrode for Dye-Sensitized Solar Cells

  • Ko, Yohan;Choi, Wooyeol;Kim, Youbin;Lee, Chanyong;Jun, Yongseok;Kim, Junhee
    • Journal of Electrochemical Science and Technology
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    • v.10 no.3
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    • pp.313-320
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    • 2019
  • In this study, cobalt diselenide ($CoSe_2$) and the composites ($CoSe_2@RGO$) of $CoSe_2$ and reduced graphene oxide (RGO) were synthesized by a facile hydrothermal reaction using cobalt ions and selenide source with or without graphene oxide (GO). The formation of $CoSe_2@RGO$ composites was identified by analysis with X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy and scanning electron microscopy (SEM). Electrochemical analyses demonstrated that the $CoSe_2@RGO$ composites have excellent catalytic activity for the reduction of $I_3{^-}$, possibly indicating a synergetic effect of $CoSe_2$ and RGO. As a consequence, the $CoSe_2@RGO$ composites were applied as a counter electrode in DSSC for the reduction of redox couple electrolyte, and exhibiting the comparable power conversion efficiency (7.01%) to the rare metal platinum (Pt) based photovoltaic device (6.77%).