• 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.

• Journal of the Korean Chemical Society
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• v.19 no.3
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• pp.174-178
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• 1975

The intermediate, 17${\alpha}$-methyl-4-aza-5${\alpha}$-androstan-17${\beta}$-ol(Ⅸ) required for the synthesis of 4-(${\beta}$-guanidinoethyl)-17${\alpha}$-methyl-4-aza-5${\alpha}$-androstan-17${\beta}$-ol(V) was obtained through a reaction of 17${\alpha}$-methyl-3,5-seco-4-norandrostan-17${\beta}$-ol-5-on-3-oic acid(VI) with ammonium hydroxide followed by two reductions(platinum dioxide with hydrogen and lithium aluminium hydride). Condensation of Ⅸ with chloroacetonitrile under anhydrous condition, followed by reduction of the nitrile with lithium aluminium hydride gave 4-(${\beta}$-aminoethyl)-17${\alpha}$-methyl-4-aza-5${\alpha}$-androstan-17${\beta}$-ol(XI). The reaction of XI with 2-methyl-2-thiopseudourea or 3,5-dimethylpyrazole-1-carboxamidine, or cyanamide provided the title compound, V. Relaxation of the nictitating membrane, in the absence of mydriasis, is considered to be evidence of adrenergic neurone blockade. Thus the test compound(V) resembles that of the classical adrenergic neurone blocking agents.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.20 no.5
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• pp.13-19
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• 2019

After the Fukushima nuclear accident, a new power supply using a lithium polymer battery has been proposed the first time in the world as the safety of the emergency battery facility has been required. It is required to have the safety of the rack system in which the battery device is installed in order to apply the proposed technology to the field. Therefore, the purpose of this study is to evaluate the seismic performance of string and rack frame for lithium-polymer battery devices developed for the first time in the world to satisfy 72 hours capacity. (1) The natural frequency of the unit rack system was 9 Hz, and the natural frequency before and after the earthquake load did not change. This means that the connection between members is secured against the design earthquake load. (2) he vibration reduction effect by string design was about 20%. (3) As a result of the seismic performance test under OBE and SSE conditions, the rack frame system was confirmed to be safe. Therefore, the proposed rack system can be applied to the nuclear power plant because the rack system has been verified structural safety to the required seismic forces.

• Korean Chemical Engineering Research
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• v.60 no.3
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• pp.446-451
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• 2022

In this study, to improve capacity and cycle stability, the pitch coated nano silicon sheets/CNT composites were prepared through electrostatic bonding of nano silicon sheets and CNT. Silica sheets were synthesized by hydrolyzing TEOS on the crystal planes of NaCl, and then nano silicon sheets were prepared by using magnesiothermic reduction method. To fabricate the nano silicon sheets/CNT composites, the negatively charged CNT after the acid treatment was used to assemble the positively charged nano silicon sheets modified with APTES. THF as a solvent was used in the coating process of PFO pitch. The physical properties of the prepared anode composites were analysed by FE-SEM, XRD and EDS. The electrochemical performances of the synthesized anode composites were performed by current charge/discharge, rate performances, differential capacity and EIS tests in the electrolyte LiPF₆ dissolve solvent (EC:DMC:EMC = 1:1:1 vol%). It was found that the anode material with high capacity and stability could be synthesized when high composition of silicon and conductivity of CNT were used. The pitch coated nano silicon sheets/CNT anode composites showed initial discharge capacity of 2344.9 mAh/g and the capacity retention ratio of 81% after 50 cycles. The electrochemical property of pitch coated anode material was more improved than that of the nano silicon sheets/CNT composites.

• Journal of the Korean Electrochemical Society
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• v.27 no.3
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• pp.88-96
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• 2024

Lithium metal has garnered attention as a promising anode active material thanks to its high specific capacity, energy density, and the lowest reduction potential. However, the formation of dendrites, dendritic crystals that arise during the charge and discharge process, has posed safety and lifetime stability challenges. To resolve this, our study has introduced a novel separator design. This separator features a composite coating of vapor-grown carbon fiber, a conductive material in nanofibers, and silver. We have meticulously studied the impact of this innovative separator on the electrochemical properties of the lithium metal anode, unveiling promising results. To confirm the synergistic effect of VGCF and Ag, a separator with no surface treatment and a separator with only VGCF coated on one side were prepared and compared with the Ag-VGCF-separator. In the case of the bare separator, the Li metal surface is covered with dendrites during the initial charge and discharge process. In contrast, both the VGCF-separator and the Ag-VGCF-separator show Li precipitation inside the conductive coating layer coated on the separator surface. Additionally, the Ag-VGCF-separator showed a more uniform precipitate shape than the VGCF-separator. As a result, the Ag-VGCF-separators show improved electrochemical properties compared to the bare separators and the VGCF-separators.

• Journal of the Korean Applied Science and Technology
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• v.20 no.1
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• pp.33-43
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• 2003

$LiMn_2O_4$ catalyst for $CO_2$ decomposition was synthesized by oxidation method for 30 min at 600$^{\circ}C$ in an electric furnace under air condition using manganese(II) nitrate $(Mn(NO_3)_2{\cdot}6H_2O)$, Lithium nitrate ($LiNO_3$) and Urea $(CO(NH_2)_2)$. The synthesized catalyst was reduced by $H_2$ at various temperatures for 3 hr. The reduction degree of the reduced catalysts were measured using the TGA. And then $CO_2$ decomposition rate was measured using the reduced catalysts. Phase-transitions of the catalysts were observed after $CO_2$ decomposition reaction at an optimal decomposition temperature. As the result of X-ray powder diffraction analysis, the synthesized catalyst was confirmed that the catalyst has the spinel structure, and also confirmed that when it was reduced by $H_2$, the phase of $LiMn_2O_4$ catalyst was transformed into $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase. After $CO_2$ decomposition reaction, it was confirmed that the peak of $LiMn_2O_4$ of spinel phase. The optimal reduction temperature of the catalyst with $H_2$ was confirmed to be 450$^{\circ}C$(maximum weight-increasing ratio 9.47%) in the case of $LiMn_2O_4$ through the TGA analysis. Decomposition rate(%) using the $LiMn_2O_4$ catalyst showed the 67%. The crystal structure of the synthesized $LiMn_2O_4$ observed with a scanning electron microscope(SEM) shows cubic form. After reduction, $LiMn_2O_4$ catalyst became condensed each other to form interface. It was confirmed that after $CO_2$ decomposition, crystal structure of $LiMn_2O_4$ catalyst showed that its particle grew up more than that of reduction. Phase-transition by reduction and $CO_2$ decomposition ; $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase at the first time of $CO_2$ decomposition appear like the same as the above contents. Phase-transition at $2{\sim}5$ time ; $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase by reduction and $LiMn_2O_4$ of spinel phase after $CO_2$ decomposition appear like the same as the first time case. The result of the TGA analysis by catalyst reduction ; The first time, weight of reduced catalyst increased by 9.47%, for 2${\sim}$5 times, weight of reduced catalyst increased by average 2.3% But, in any time, there is little difference in the decomposition ratio of $CO_2$. That is to say, at the first time, it showed 67% in $CO_2$ decomposition rate and after 5 times reaction of $CO_2$ decomposition, it showed 67% nearly the same as the first time.

• 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 $400{\mu}Ah/cm^2$.

• Resources Recycling
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• v.32 no.6
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• pp.25-33
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• 2023

With the growth of the battery industry, a rapid increase in the production and usage of lithium-ion batteries is expected, and in line with this, much interest and effort is being paid to recycle waste batteries, including production scrap. Although much effort has been made to recycle cathode material, much attention has begun to recycle anode material to secure the supply chain of critical minerals and improve recycling rates. The proximate analysis that measures the content of coal can be used to analyze graphite in anode material, but it cannot accurately analyze due to the interaction between the components of the black mass. Therefore, in this study, thermogravimetric analysis of each component of black mass was measured as the temperature increased up to 950℃ in an oxygen atmosphere. As a result, in the case of cathode material, no change in mass was measured other than a mass reduction of about 5% due to oxidation of the binder and conductive material. In the case of anode material, except for a mass reduction of about 2% due to the binder, all mass reduction were due to the graphite(fixed carbon). In addition, metal conductors (Al, Cu) were oxidized and their mass increased as the temperature increased. Thermal analysis results of mixed samples of cathode/anode show similar results to the predictive values that can be calculated through each cathode and anode analysis results.

• Clean Technology
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• v.24 no.1
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• pp.77-84
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• 2018

In this study, $Li_4Ti_5O_{12}$ anode materials for lithium ion battery were synthesized by dry ball-mill method. Polyvinyl chloride (PVC) as a carbon source was added to improve electrochemical properties. When the PVC was added after $Li_4Ti_5O_{12}$ formation, the spinel structure was well synthesized and it was confirmed by X-ray diffraction (XRD) experiments. When the carbon material was added before the synthesis and the heat treatment was performed, it was confirmed that a material having a different crystal structure was synthesized even when a small amount of carbon material was added. In the case of $Li_4Ti_5O_{12}$ without the carbon material, the electrical conductivity value was about $10{\mu}S\;m^{-1}$, which was very small and similar to that of the nonconductor. As the carbon was added, the electrical conductivity was greatly improved and increased up to 10,000 times. Electrochemical impedance spectroscopy (EIS) analysis showed that the size of semicircle corresponding to the resistance decreased with the carbon addition. This indicates that the resistance inside the electrode is reduced. According to the Cyclic voltammetry (CV) analysis, the potential difference between the oxidation peak and the reduction peak was reduced with carbon addition. This means that the rate of lithium ion insertion and deinsertion was increased. $Li_4Ti_5O_{12}$ with 9.5 wt% PVC added sample showed the best properties in rate capabilities of $180mA\;h\;g^{-1}$ at 0.2 C-rate, $165mA\;h\;g^{-1}$ at 0.5 C-rate, and $95.8mA\;h\;g^{-1}$ at 5 C-rate.

• Journal of the Korean Electrochemical Society
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• v.11 no.2
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• pp.100-104
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• 2008

Titanium sheet metal substrates used in thin film batteries were wet etched and their surface area was increased in order to increase the discharge capacity and power density of the batteries. To obtain a homogeneous etching pattern, we used a conventional photolithographic process. Homogeneous hemisphere-shaped wells with a diameter of approximately $40\;{\mu}m$ were formed on the surface of the Ti substrate using a photo-etching process with a $20\;{\mu}m{\times}20\;{\mu}m$ square patterned photo mask. All-solid-state thin film cells composed of a Li/Lithium phosphorous oxynitride (Lipon)/$LiCoO_2$ system were fabricated onto the wet etched substrate using a physical vapor deposition method and their performances were compared with those of the cells on a bare substrate. It was found that the discharge capacity of the cells fabricated on wet etched Ti substrate increased by ca. 25% compared to that of the cell fabricated on bare one. High discharge rate was also able to be obtained through the reduction in the internal resistance. However, the cells fabricated on the wet etched substrate exhibited a higher degradation rate with charge-discharge cycling due to the nonuniform step coverage of the thin films, while the cells on the bare substrate demonstrated a good cycling performance.