• Applied Chemistry for Engineering
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• v.26 no.6
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• pp.674-680
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• 2015

A solvent-soluble polyimide (PI) polymeric binder was synthesized by a two-step reaction for silicon (Si) anodes for lithium-ion batteries. Polyamic acid was first prepared through ring opening between two monomers, bicyclo[2,2,2]oct-7-ene-2,3,5,6-tetracarboxylic dianhydride (BCDA) and 4,4-oxydianiline (ODA), followed by condensation reaction. Using the synthesized PI polymeric binder (molecular weight = ~10,945), the coating slurry was then prepared and Si anode was fabricated. For the control system, Si anode based on polyvinylidene fluoride (PVDF, molecular weight = ~350,000) having the same constituent ratio was prepared. During precycling, PI polymeric binder revealed much improved discharge capacity ($2,167mAh\;g^{-1}$) compared to that of using PVDF polymeric binder ($1,740mAh\;g^{-1}$), while the Coulombic efficiency of two systems were similar. PI polymeric binder improved the cycle retention ability during cycles compared to that of using PVDF, which is attributed to an improved adhesion property inside Si anode diminishing the dimensional stress during Si volume changes. The adhesion property of each polymeric binder in Si anode was confirmed by surface and interfacial cutting analysis system (SAICAS) (Si anode based on PI polymeric binder = $0.217kN\;m^{-1}$ and Si anode based on PVDF polymeric binder = $0.185kN\;m^{-1}$).

• Applied Chemistry for Engineering
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• v.33 no.5
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• pp.496-501
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• 2022

In this study, an anode material for lithium secondary batteries was manufactured using petroleum-based residual oil, which is a petroleum refining by-product. Among petroleum-based residual oils, pyrolysis fuel oil (PFO), fluidized catalyst cracking-decant oil (FCC-DO), and vacuum residue (VR) were used as carbon precursors. The physicochemical characteristics of petroleum-based residual oil were confirmed through Matrix-assisted laser desorption/ionization Time-of-Flight (MALDI-TOF) and elemental analysis (EA), and the structural characteristics of anode materials manufactured from residual oil were evaluated using X-ray crystallography (XRD) and Raman spectroscopic techniques. VR was found to contain a wide range of molecular weight distributions and large amounts of impurities compared to PFO and FCC-DO, and PFO and FCC-DO exhibited almost similar physicochemical characteristics. From the XRD analysis results, carbonized PFO and FCC-DO showed similar d₀₀₂ values. However, it was confirmed that FCC-DO had a more developed layered structure than PFO in Lc (Length of a and c axes in the crystal system) and La values. In addition, FCC-DO showed the best cycle characteristics in electrochemical characteristics evaluation. According to the physicochemical and electrochemical results of the petroleum-based residual oil, FCC-DO is a better carbon precursor for a lithium secondary battery than PFO and VR.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2002.11a
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• pp.210-215
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• 2002

This thesis is contents on the crystal grown by the solide phase method at $925^{\circ}C$ with orthorhombic structure that $LiMnO_{2}$ active material synthesised with precurse $Mn_{2}O_{3}$ and $LiOH.H_{2}O$ material to get three voltage level. The porosity analysis of the grown crystal in secondary batteries $LiMnO_{2}$ thin film is $1.323E+02\AA$ of the average pore diameter of powder particles and its structure to be taken the pore diameter was prepared. Adding voltage area to get properties of charge and discharge of which experiment result of $LiMnO_{2}$ thin film area 2.2V~4.3V, current and scan speed were 0.1mAh/g and $0.2mV/cm^{2}$ respectively, and properties of the charge and discharge to be got optimum experiment condition parameter and density rate of Li for analyze that unit discharge capacity with metal properties is 87mAh/g was 96.9[ppm] at 670.784[nm] wavelength, and density rate of Mn analyzed 837[ppm] at 257.610[nm]. It can be estimated the quality of thin film that wrong cell reject from the bottle of electrolyte. The results of SEM and XRD were the same that of original researchers.

• Journal of the Korean Electrochemical Society
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• v.17 no.3
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• pp.149-155
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• 2014

In this study, a positive-electrode material in a lithium secondary battery $Li[Ni_{0.575}Co_{0.1}Mn_{0.325}]O_2$ was synthesized as precursor by co-precipitation. Cathode material was synthesized by adding iron. The synthesized cathode material was analyzed by scanning electron microscope and x-ray diffraction. The analysis of x-ray diffraction showed that the a-axis and c-axis is increased by doping iron. And $I_{(003)}/I_{(104)}$ is increased and $I_{(006)}+I_{(102)}/I_{(101)}$ is decreased. Through this result, it was confirmed that the structural stability is improved. And impedance measurements show that the charge transfer resistance ($R_{ct}$) is lowered by doping iron. Consequently, electrochemical properties are improved by doping iron. In particular, the cycle characteristics are improved at a high temperature condition (328 K). Structural stabilities are contributing to the cycle properties.

• Journal of the Korean Society of Safety
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• v.38 no.5
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• pp.8-14
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• 2023

Lithium ions can induce the thermal runaway phenomenon and lead to reignition due to electrical, mechanical, and environmental factors such as high temperature, smoke generation, explosions, or flames, which is extremely likely to create safety concerns. Therefore, one of the ways to improve the flame retardancy of the electrolyte is to use a flame-retardant additive. Comparing the associated characteristic value of existing substances with the required experimental value, it was found that these values were either considerably different or were not documented. It is vital to know a substance's combustion characteristic values, flash point, explosion limit, and autoignition temperature (AIT) as well as its combustion characteristics before using it. In this research, the flash point and AIT of materials were measured by mixing a highly volatile and flammable substance, diethyl carbonate (DEC), with flame-retardant dimethyl methylphosphonate (DMMP). The flash point of DEC, which is a pure substance, was 29℃, and that for DMMP was 65℃. Further, the lower explosion limit calculated using the measured flash point of DEC was 1.79 Vol.%, while that for DMMP was 0.79 Vol.%. The AIT was 410℃ and 390℃ for DEC and DMMP, respectively. In particular, since the AIT of DMMP has not been discussed in any previous study, it is necessary to ensure safety through experimental values. In this study, the experimental and regression analysis revealed that the average absolute deviation (ADD) for the flash point of the DEC+DMMP DEC+DMMP system is 0.58 sec and that the flash point tends to increase according to changes in the composition employed. It also revealed that the AAD for the AIT of the mixture was 3.17 sec and that the AIT tended to decrease and then increase based on changes in the composition.

• Journal of the Korean Electrochemical Society
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• v.22 no.1
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• pp.36-42
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• 2019

A macroporous Sn thick film as a high capacity negative electrode for a lithium ion secondary battery was prepared by using a chemical etching method using nitric acid for a Sn film having a thickness of $52{\mu}m$. The porous Sn thick film greatly reduced the over-voltage for the alloying reaction with lithium by the increased reaction area. At the same time. The porous structure of active Sn film plays a part in the buffer and reduces the damage by the volume change during cycles. Since the porous Sn thick film electrode does not require the use of the binder and the conductive carbon black, it has substantially larger energy density. As the concentration of nitric acid in etching solution increased, the degree of the etching increased. The etching of the Sn film effectively proceeded with nitric acid of 3 M concentration or more. The porous Sn film could not be recovered because the most of Sn was eluted within 60 seconds by the rapid etching rate in the 5 M nitric acid. In the case of etching with 4 M nitric acid for 60 seconds, the appropriate porous Sn film was formed with 48.9% of weight loss and 40.3% of thickness change during chemical acid etching process. As the degree of etching of Sn film increased, the electrochemical activity and the reversible capacity for the lithium storage of the Sn film electrode were increased. The highest reversible specific capacity of 650 mAh/g was achieved at the etching condition with 4 M nitric acid. The porous Sn film electrode showed better cycle performance than the conventional electrode using a Sn powder.

• Applied Chemistry for Engineering
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• v.32 no.1
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• pp.83-90
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• 2021

In this study, effects of the physical and chemical properties of low temperature heated carbon on electrochemical behavior as a secondary battery anode material were investigated. A heat treatment at 600 ℃ was performed for coking of petroleum based pitch, and the manufactured coke was heat treated with different heat temperatures at 700~1,500 ℃ to prepare low temperature heated anode materials. The physical and chemical properties of carbon anode materials were studied through nitrogen adsorption and desorption, X-ray diffraction (XRD), Raman spectroscopy, elemental analysis. Also the anode properties of low temperature heated carbon were considered through electrochemical properties such as capacity, initial Coulomb efficiency (ICE), rate capability, and cycle performance. The crystal structure of low temperature (≤ 1500 ℃) heated carbon was improved by increasing the crystal size and true density, while the specific surface area decreased. Electrochemical properties of the anode material were changed with respect to the physical and chemical properties of low temperature heated carbon. The capacity and cycle performance were most affected by H/C atomic ratio. Also, the ICE was influenced by the specific surface area, whereas the rate performance was most affected by true density.

• Journal of the Korean Electrochemical Society
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• v.14 no.4
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• pp.208-213
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• 2011

Solid polymer electrolytes using $BF_3LiMA$ as monomer were synthesized by usual one step radical polymerization in THF solvent. The effect of $BF_3LiMA$ concentration on ionic conductivity and electrochemical stability was investigated by AC impedance measurement and linear sweep voltammetry. As a result, the highest ionic conductivity reached $7.71{\times}10^{-6}S\;cm^{-1}$ at $25^{\circ}C$ was obtained in 12.9 wt% of $BF_3LiMA$ content. Further increase or decrease of $BF_3LiMA$ content result to decrease the ionic conductivity due to the brittle matrix properties in former case and the insufficient number of charge carrier in the latter case. Furthermore, since the counter-anion was immobilized in the self-doped solid polymer electrolytes, high electrochemical stability up to 6.0 V was observed even in $60^{\circ}C$.

• Journal of the Korean Electrochemical Society
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• v.17 no.1
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• pp.65-70
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• 2014

In this study, crosslinked poly(POEM-co-AMPSLi-co-GMA)s were prepared by epoxy coupling of GMA after radical copolymerization of AMPS, POEM and GMA followed by acid-base titration reaction between sulfonic acid of AMPS and $Li_2CO_3$. It was observed that the crystalline melting temperature of POEM was effected by mol% of components and shifted to lower value by lithiation of AMPS group. The ionic conductivity of crosslinked polymer electrolyte was decreased by addition of GMA but maintained over $1.0{\times}10^{-6}S\;cm^{-1}$ until 16 mol%. Particularly, the self-doped polymer electrolyte with 2 mol% of GMA showed its ionic conductivity as high as $4.08{\times}10^{-6}S\;cm^{-1}$ at room temperature and electrochemical stability up to 6 V. In addition, 0.11 MPa of modulus and 270% of elongation were obtained from the free standing film of crosslinked polymer electrolyte.

• Journal of the Korean Chemical Society
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• v.63 no.6
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• pp.446-452
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• 2019

We have developed a method that can leach Co, Mn, and Ni in the cathode active material safely using lactic acid. When cathode active material was leached by lactic acid, lactic acid showed the highest efficiency at 2 N than 1 N and above 4 N concentration. When the cathode active material was added incrementally into the solution of lactic acid, the maximum solubility was 30 g/L at 2 N concentration. Oxalic acid was added in the solution of lactic acid and it showed that rare metals represent the most economical recovery efficiency at 4 g/L. Based on this study, it was found that the optimal condition for recovery of rare metals from cathode active material is oxalic acid : cathode active material = 7 : 1 as a ratio of weight. In addition, it was observed that the precipitate produced by oxalic acid is a polynuclear crystalline material bonded with 3 components of Co, Ni, and Mn.