• Carbon letters
• /
• v.16 no.4
• /
• pp.233-240
• /
• 2015

Electrochemical synthesis was employed to prepare a novel hydroxyapatite/graphene (HAP/Gr) composite powder suitable for medical applications as a hard tissue implant (scaffold). The synthesis was performed in a homogeneous dispersion containing Na₂H₂EDTA·2H₂O, NaH₂PO₄ and CaCl₂ with a Ca/EDTA/PO₄³⁻ concentration ratio of 0.25/0.25/0.15M, along with 0.01 wt% added graphene nanosheets, at a current density of 137 mA cm⁻² and pH value of 9.0. The field emission scanning electron microscopy and transmission electron microscopy observations of the composite HAP/Gr powder indicated that nanosized hydroxyapatite particles were uniformly placed in the graphene overlay. Raman spectroscopy, Fourier transform infrared spectroscopy and X-ray diffraction confirmed graphene incorporation in the HAP/Gr powder. The electrochemically prepared HAP/Gr composite powder exhibited slight antibacterial effect against the growth of the bacterial strain Staphylococcus aureus.

• Journal of Powder Materials
• /
• v.23 no.4
• /
• pp.317-324
• /
• 2016

Tin is one of the most promising anode materials for next-generation lithium-ion batteries with a high energy density. However, the commercialization of tin-based anodes is still hindered due to the large volume change (over 260%) upon lithiation/delithiation cycling. To solve the problem, many efforts have been focused on enhancing structural stability of tin particles in electrodes. In this work, we synthesize tin nano-powders with an amorphous carbon layer on the surface and surroundings of the powder by electrical wire explosion in alcohol-based liquid media at room temperature. The morphology and microstructures of the powders are characterized by scanning electron microscopy, X-ray diffraction, Raman spectroscopy, and transmission electron microscopy. The electrochemical properties of the powder for use as an anode material for lithium-ion battery are evaluated by cyclic voltammetry and a galvanometric discharge-charge method. It is shown that the carbon-coated tin nano-powders prepared in hexanol media exhibit a high initial charge specific capacity of 902 mAh/g and a high capacity retention of 89% after 50 cycles.

• Journal of Electrochemical Science and Technology
• /
• v.9 no.4
• /
• pp.260-275
• /
• 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.

• Journal of Surface Science and Engineering
• /
• v.55 no.3
• /
• pp.143-155
• /
• 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.

• Journal of Electrochemical Science and Technology
• /
• v.7 no.2
• /
• pp.170-178
• /
• 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.

• Advances in nano research
• /
• v.5 no.3
• /
• pp.215-230
• /
• 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.

• Journal of Electrochemical Science and Technology
• /
• v.14 no.1
• /
• pp.21-30
• /
• 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.

• Transactions of the Korean Society of Mechanical Engineers A
• /
• v.31 no.10
• /
• pp.986-992
• /
• 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.

• Journal of Electrochemical Science and Technology
• /
• v.10 no.4
• /
• pp.361-372
• /
• 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.

• Journal of Electrochemical Science and Technology
• /
• v.12 no.1
• /
• pp.112-125
• /
• 2021

The new emerging "High entropy materials" attract the attention of the scientific society because of their simpler structure and spectacular applications in many fields. A novel nanocrystalline high entropy (Be,Mg,Ca,Sr,Zn,Ni)3O4 oxide has been successfully synthesized through mechanochemical treatment followed by sintering and air quenching. The present research work focuses on the possibility of single-phase formation in the aforementioned high entropy oxide despite the great difference in the atomic sizes of reactant alkaline earth and 3d transition metal oxides. Structural properties of (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide were explored by confirmation of its single-phase Fd-3m spinel structure by x-ray diffraction (XRD). Further, nanocrystalline nature and morphology were analyzed by scanning electron microscopy (SEM). Among thermal properties, thermogravimetric analysis (TGA) revealed that the (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide is thermally stable up to a temperature of 1200℃. Whereas phase evolution in (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide before and after sintering was analyzed through differential scanning calorimetry (DSC). Electrochemical studies of (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide consists of a comparison of thermodynamic and kinetic parameters of water and hydrazine hydrate oxidation. Values of activation energy for water oxidation (9.31 kJ mol-1) and hydrazine hydrate oxidation (13.93 kJ mol-1) reveal that (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide is catalytically more active towards water oxidation as compared to that of hydrazine hydrate oxidation. Electrochemical impedance spectroscopy is also performed to get insight into the kinetics of both types of reactions.