• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.19 no.7
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• pp.650-654
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• 2006

[ $LiNi_{0.4}Mn_{0.3}Co_{0.3}O_2$ ] cathode material was synthesized by a mixed hydroxide method. Structural characterization was carried out using X-ray diffraction studies. Electrochemical studies were performed by assembling 2032 coin cells with lithium metal as an anode. DSC (Differential scanning calorimetry) data showed that exothermic reactions of $LiNi_{0.4}Mn_{0.3}Co_{0.3}O_2$ charged to 4.3 V versus Li started at high temperatures$(280\sim390^{\circ}C)$. The cell of $LiNi_{0.4}Mn_{0.3}Co_{0.3}O_2$ mixed cathode delivered a discharge capacity of 150 mAh/g at a 0.2 C rate. The capacity of the cell decreased with the current rate and a useful capacity of 134 mAh/g was obtained at a 2 C rate. The reversible capacity after 100th cycles was 126 mAh/g when a cell was cycled at a current rate of 0.5 C in $2.8\sim4.3V$.

• Journal of Powder Materials
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• v.23 no.2
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• pp.136-142
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• 2016

As precursors of cathode materials for lithium ion batteries, $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$ powders are prepared in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH in the presence of $NH_4OH$ in air or nitrogen ambient. Calcination of the precursors with $Li_2CO_3$ for 8 h at $1,000^{\circ}C$ in air produces dense spherical cathode materials. The precursors and final powders are characterized by X-ray diffraction (XRD), scanning electron microscopy, particle size analysis, tap density measurement, and thermal gravimetric analysis. The precursor powders obtained in air or nitrogen ambient show XRD patterns identified as $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$. Regardless of the atmosphere, the final powders exhibit the XRD patterns of $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ (NCM). The precursor powders obtained in air have larger particle size and lower tap density than those obtained in nitrogen ambient. NCM powders show similar tendencies in terms of particle size and tap density. Electrochemical characterization is performed after fabricating a coin cell using NCM as the cathode and Li metal as the anode. The NCM powders from the precursors obtained in air and those from the precursors obtained in nitrogen have similar initial charge/discharge capacities and cycle life. In conclusion, the powders co-precipitated in air can be utilized as precursor materials, replacing those synthesized in the presence of nitrogen injection, which is the usual industrial practice.

• Bulletin of the Korean Chemical Society
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• v.27 no.8
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• pp.1175-1180
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• 2006

Si-C composites were prepared by the carbonization of polyaniline (PAn) coated on silicone powder. The physical and electrochemical properties of the Si-C composites were characterized by particle-size analysis, X-ray diffraction, scanning electron microscopy, and battery electrochemical tests. The average particle size of Si was increased by the coating of Pan but somewhat reduced by the carbonization to give silicone-carbon composites. The co-existence of crystalline silicone and amorphous-like carbon was confirmed by XRD analyses. SEM photos showed that the silicone particles were well covered with carbonaceous materials, depending on the PAn content. Si-C$\mid$Li cells were fabricated using the Si-C composites and tested using galvanostatic charge-discharge. Si-C$\mid$Li cells gave better electrochemical properties than Si|Li cells. Si-C$\mid$Li cells using Si-C from HCl-undoped precursor PAn showed better electrochemical properties than precursor PAn doped in HCl. The addition of an electrolyte containing 4-fluoroethylene carbonate (FEC) increased the initial discharge capacity. Also, another electrochemical test, the galvanostatic charge-discharge test with GISOC (gradual increasing of the state of charge) was carried out. Si-C(Si:PAn = 50:50 wt. ratio)|Li cell showed 414 mAh/g of reversible specific capacity, 75.7% of IIE (initial intercalation efficiency), 35.4 mAh/g of IICs (surface irreversible specific capacity).

• Korean Chemical Engineering Research
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• v.61 no.3
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• pp.348-355
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• 2023

Magnesium secondary batteries are attracting much attention due to their potential to replace conventionally used lithium ion batteries. Magnesium secondary battery cathode material Mo₆S₈ were synthesized by molten salt synthesis method and PVC as a carbon materials were added to improve electrochemical properties. Crystal structure, size and surface of the synthesized anode materials were measured through XRD and SEM. Charge-discharge profiles and rate capabilities were measured by battery test system. 2.81 wt% PVC coated sample showed the best rate capabilities of 85.8 mAh/g at 0.125 C-rate, 69.2 mAh/g at 0.5 C-rate, and 60.5 mAh/g at 1 C-rate.

• Resources Recycling
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• v.31 no.6
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• pp.81-91
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• 2022

The use of lithium-ion batteries increases significantly with the rapid spread of electronic devices and electric vehicle and thereby an increase in the amount of waste batteries is expected in the near future. Therefore, studies are continuously being conducted to recover various resources of cathode active material (Ni, Co, Mn, Li) from waste battery. In order to recover the cathode active material, black mass is generally recovered from waste battery. The general process of recovering black mass is a waste battery collection - discharge - dismantling - crushing - classification process. This study focus on the crushing/classification process among the processes. Specifically, the particle size distribution of various samples at each crushing/classification step were evaluated, and the particle shape of each particle fraction was analyzed with a microscope and SEM (Scanning Electron Microscopy)-EDS(Energy Dispersive Spectrometer). As a result, among the black mass particle, fine particle less than 74 ㎛ was the mixture of cathode and anode active material which are properly liberated from the current metals. However, coarse particle larger than 100 ㎛ was present in a form in which the current metal and active material were combined. In addition, this study developed a PBM(Population Balance Model) system that can simulate two-species mixture sample with two different crushing properties. Using developed model, the breakage parameters of two species was derived and predictive performance of breakage distribution was verified.

• Journal of the Korean Electrochemical Society
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• v.11 no.4
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• pp.284-288
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• 2008

Sn-thin film as high capacitive anode for thin film lithium-ion battery was prepared by organic-electrolyte electroplating using Sn(II) acetate. Electrolytic solution including $Li^+$ and $Sn^{2+}$ had 3 reduction peaks at cyclic voltammogram. Current peak at $2.0{\sim}2.5\;V$ region correspond to the electroplating of Sn on Ni substrate. This potential value is lower than 2.91 V vs. $Li^+/Li^{\circ}$, of the standard reduction potential of $Sn^{2+}$ under aqueous media. It is the result of high overpotential caused by high resistive organic electrolytic solution and low $Sn^{2+}$ concentration. Physical and electrochemical properties were evaluated using by XRD, FE-SEM, cyclic voltammogram and galvanostatic charge-discharge test. Crystallinity of electroplated Sn-anode on a Ni substrate could be increased through heat treatment at $150^{\circ}C$ for 2 h. Cyclic voltammogram shows reversible electrochemical reaction of reduction(alloying) and oxidation(de-alloying) at 0.25 V and 0.75 V, respectively. Thickness of Sn-thin film, which was calculated based on electrochemical capacity, was $7.35{\mu}m$. And reversible capacity of this cell was $400{\mu}Ah/cm^2$.

• Journal of the Korean Electrochemical Society
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• v.17 no.2
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• pp.86-93
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• 2014

Mesoporous tin oxide (meso-$SnO_2$) with 5 nm mesopore and well-aligned $SnO_2$ nanowire-bundles with 5~7 nm diameters were prepared by template synthesis method. In addition to meso-$SnO_2$, meso-$SnO_2$/$SiO_2$, which has almost the same structure as meso-$SnO_2$ including $SiO_2$ used as the template were prepared by the modification of template synthesis. X-ray diffraction, N2 adsorption-desorption isotherms, transmission electron microscopy observed structures of meso-$SnO_2$ and meso-$SnO_2$/$SiO_2$. Although the meso-$SnO_2$/$SiO_2$ showed some positive evidences to suppress the volume change of meso-$SnO_2$ through cyclic voltammogram, electrochemical impedance spectroscopy, and voltage profiles during cycling, its cycle life was not improved highly to address modified structural effects. Thus, further study might be done to control the nanostructure of meso-$SnO_2$/$SiO_2$ for enhanced cycle performance.

• Journal of the Korean Electrochemical Society
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• v.12 no.2
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• pp.189-195
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• 2009

$\beta-Ga_{2}O_{3}$ nanorods were synthesized by chemical vapor deposition method using nickel-oxide nanoparticle as a catalyst and gallium metal powder as a source material. The average diameter of nanorods was around 160 nm and the average length was $4{\mu}m$. Also, we confirmed that the synthesis of nanorods follows the vapor-solid growth mechanism. From the results of X-ray diffraction and HR-TEM observation, it can be found that the synthesized nanorods consisted of a typical core-shell structure with single-crystalline $\beta-Ga_{2}O_{3}$ core with a monoclinic crystal structure and an outer amorphous gallium oxide layer. Li/$\beta-Ga_{2}O_{3}$ nanorods cell delivered capacity of 867 mAh/g-$\beta-Ga_{2}O_{3}$ at first discharge. Although the Li/$\beta-Ga_{2}O_{3}$ nanorods cell showed low coulombic efficiency at first cycle, the cell exhibited stable cycle life property after fifth cycle.

• Korean Chemical Engineering Research
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• v.58 no.1
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• pp.142-149
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• 2020

In this study, the electrochemical performance of Graphite/Silicon/Pitch composites as anode material was investigated to improve the low theoretical capacity of artificial graphite. Spherical artificial graphite surface was coated with polyvinylpyrrolidone (PVP) amphiphiles material to synthesize Graphite/Silica material by silica islands growth. The Graphite/Silicon/Pitch composites were prepared by petroleum pitch coating and magnesiothermic reduction. The Graphite/Silicon/Pitch composite electrodes manufactured using poly(vinylidene fluoride) (PVDF), carboxymethyl cellulose (CMC) and polyacrylic acid (PAA) binders. The coin type half cell was assembled using various electrolytes and additives. The Graphite/Silicon/Pitch composites were analysed by X-ray diffraction (XRD), scanning electron microscope (SEM) and a thermogravimetric analyzer (TGA). The electrochemical characteristics of Graphite/Silicon/Pitch composite were investigated by constant current charge/discharge, rate performance, cyclic voltammetry and electrochemical impedance spectroscopy. The Graphite/Silicon/Pitch composites showed high cycle stability at a graphite/silica/pitch ratio (1:4:8 wt%). When the electrode is prepared using PAA binder, the high capacity and stability is obtained. The coin type half cell assembled using EC: DMC: EMC electrolyte showed high initial capacity (719 mAh/g) and excellent cycle stability. The rate performance has an capacity retention (77%) at 2 C/0.1 C and an capacity recovery (88%) at 0.1 C / 0.1 C when the vinylene carbonate (VC) was added.

• Bulletin of the Korean Chemical Society
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• v.21 no.11
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• pp.1125-1132
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• 2000

The pH effect of the precursor solution on the preparation of $LiCoO_2$ by a solution phase reaction containing malonic acid was carried out. Layered $LiCoO_2$ powders were obtained with the precursors prepared at the different pHs (4, 7, and 9) and heat-treated at $700^{\circ}C(LiCoO_2-700)$ or $850^{\circ}C(LiCoO_2-850)$ in air. pHs of the media for precursor synthesis affects the charge/discharge and electrochemical properties of the $LiCoO_2electrodes.$ Upon irrespective of pH of the precursor media, X-ray diffraction spectra recorded for $LiCoO_2-850$ powder showed higher peak intensity ratio of I(003)/I(104) than that of $LiCoO_2-700$, since the better crystallization of the former crystallized better. However, $LiCoO_2$ synthesized at pH 4 displayed an abnormal higher intensity ratio of I(003)/I(104) than those synthesized at pH 7 and 9. The surface morphology of the $LiCoO_2-850$ powders was rougher and more irregular than that of $LiCoO_2-700$ made from the precursor synthesized at pH 7 and 9. The $LiCoO_2electrodes$ prepared with the precursors synthesized at pH 7 and 9 showed a better electrochemical and charge/discharge characteristics. From the AC impedance spectroscopic experiments for the electrode made from the precursor prepared in pH 7, the chemical diffusivity of Li ions (DLi+) in $Li0.58CoO_2determined$ was 2.7 ${\times}$10-8 $cm^2s-1$. A cell composed of the $LiCoO_2-700$ cathode prepared in pH 7 with Lithium metal anode reveals an initial discharge specific capacity of 119.8 mAhg-1 at a current density of 10.0 mAg-1 between 3.5 V and 4.3 V. The full-cell composed with $LiCoO_2-700$ cathode prepared in pH 7 and the Mesocarbon Pitch-based Carbon Fiber (MPCF) anode separated by a Cellgard 2400 membrane showed a good cycleability. In addition, it was operated over 100 charge/discharge cycles and displayed an average reversible capacity of nearly 130 mAhg-1.