• Bulletin of the Korean Chemical Society
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• v.32 no.2
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• pp.536-540
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• 2011

This study reports the origin of the electrochemical improvement of $LiFePO_4$ when synthesized by wet milling using acetone without conventional carbon coating. The wet milled $LiFePO_4$ delivers 149 $mAhg^{-1}$ at 0.1 C, which is comparable to carbon coated $LiFePO_4$ and approximately 74% higher than that of dry milled $LiFePO_4$, suggesting that the wet milling process can increase the capacity in addition to conventional carbon coating methods. UV spectroscopy, elemental microanalysis, and evolved gas analysis are used to find the root cause of the capacity improvement during the mechanochemical reaction in acetone. The analytical results show that the improvement is attributed to the conductive residual carbon on the surface of the wet milled $LiFePO_4$ particles, which is produced by the reaction of $FeC_2O_4{\cdot}2H_2O$ with acetone during wet milling through oxygen deficiency in the precursor.

• Journal of the Korean Electrochemical Society
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• v.2 no.3
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• pp.156-162
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• 1999

Various types of iron oxide based materials as a cathode of lithium secondary battery have been prepared and their electrochemical characteristics have been also observed. In order to understand the fundamental characteristics of iron oxide electrode, three kinds of iron oxides such as iron oxides formed by direct oxidation of iron plate or iron powders and FeOOH powders were tested with cyclic voltammetry. The oxidation and reduction peaks due to the reaction of intercalation and deintercalation were not observed for the iron oxide prepared with iron plate and FeOOH powders. In case of iron oxide prepared from iron powders, only one reduction peak was observed. A layered form of $LiFeO_2$ was synthesized directly from $FeCl_3\cdot6H_2O,\;NaOH\;and\;LiOH$ and LiOH by hydrothermal reaction. The effect of NaOH on the electrode performance was examined. When increasing NaOH, it provides the electrode with less discharge capacity and efficiency, however, decreasing rate of discharge capacity became smaller. $LiFeO_2$ synthesized with the molar ratio of $NaOH/FeCl_3/LiOH$, 2/1/7 showed the largest capacity, but the discharging efficiency was sharply decreased after 30 cycles.

• Proceedings of the Korean Magnestics Society Conference
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• 1998.05a
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• pp.68-69
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• 1998

• Bulletin of the Korean Chemical Society
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• v.30 no.8
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• pp.1719-1723
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• 2009

The LiFeP$O_4$ powder was synthesized by using the solid state reaction method with Fe($C_2O_4){\cdot}2H_2O,\;(NH_4)_2HPO_4,\;Li_2CO_3$, and chitosan as a carbon precursor material for a cathode of a lithium-ion battery. The chitosan added LiFePO4 powder was calcined at 350 ${^{\circ}C}$ for 5 hours and then 800 ${^{\circ}C}$ for 12 hours for the calcination. Then we calcined again at 800 ${^{\circ}C}$ for 12 hours. We characterized the synthesized compounds via the crystallinity, the valence states of iron ions, and their shapes using TGA, XRD, SEM, TEM, and XPS. We found that the synthesized powders were carbon-coated using TEM images and the iron ion is substituted from 3+ to 2+ through XPS measurements. We observed voltage characteristics and initial charge-discharge characteristics according to the C rate in LiFeP$O_4$ batteries. The obtained initial specific capacity of the chitosan added LiFeP$O_4$ powder is 110 mAh/g, which is much larger than that of LiFeP$O_4$ only powder.

• Journal of the Korean Chemical Society
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• v.39 no.6
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• pp.446-452
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• 1995

Lithium intercalates, $Li_xFeMoO_4Cl$ ($1{\leq}X{\leq}2$) prepared by electrochemical lithiation of $FeMoO_4Cl$ crystallizes in monoclinic structure for all x values as revealed by x-ray diffraction and galvanostatic discharge experiments. According to the x-ray photoelectron spectroscopic study, Fe(III) is at first reduced to Fe(II) upon lithium intercalation with the x domain of $0{\leq}X{\leq}1$, where the crystal symmetry is changed from tetragonal to monoclinic. On the other hand, Mo(VI) is reduced to lower valent state upon further lithium intercalation ($1{\leq}X{\leq}2$), where no crystal symmetry transformation and reduction of Fe(II) to lower valent state are observed. The Mo 3d spectrum for $Li_2FeMoO_4Cl$ appears as a complex shape, but can be deconvoluted into the three sets of the doublet on the basis of Gaussian function, those which correspond to Mo(VI), Mo(V) and Mo(IV) states, respectively. The mixed valent states of molybdenum after further lithiation may be due to a competitive reaction between the formation of Mo(V) and its disproportionation to Mo(IV) and Mo(VI).

• Journal of the Korean Electrochemical Society
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• v.11 no.3
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• pp.197-210
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• 2008

The cathode materials for lithium ion battery have been developed in accordance with the battery performance. $LiCoO_2$ initially adapted at lithium ion battery is going to be useful even at the charging voltage of 4.3 V by surface treatment or doping which drastically improved the performance of $LiCoO_2$. On the other hand, the complicate and multiple functions of recent electronic equipments required higher operational voltage and higher capacity than ever, which is going to be driving force for developing new cathode materials. Some of them are $LiNi_{1-x}{M_xO_2}$, $Li[Ni_{x}Mn_{y}Co_{z}]O_{2}$, $Li[{Ni}_{1/2}{Mn}_{1/2}]O_{2}$. Other new type of cathode materials having high safety is also developed to apply for HEV (hybrid electrical vehicle) and power tool applications. ${LiMn}_{2}{O}_{4}$ and $LiFePO_4$ are famous for highly stable material, which are expected to give contribution to make safer battery. In near future, the various materials having both capacity and safety will be developed by new technology, such as solid solution composite.

• Journal of the Korean Magnetics Society
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• v.13 no.4
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• pp.171-175
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• 2003

Electron paramagnetic resonance (EPR) of Fe$^{3+}$ in LiTaO$_3$ single crystal, grown by Czochralski method, has been studied by employing an X-band spectrometer. Resonance spectra of Fe$^{3+}$ ion on the crystallographic principal axes were obtained with 9.447 ㎓ at room temperature. The spectroscopic splitting parameter g and zero-field splitting (ZFS) parameter D (= 3 B$_{2}$sup 0/) are calculated with effective spin Hamiltonian. Fe$^{3+}$ center in stoichometric single crystal turns out to be different with that in congruent single crystal reported previously. From the analysis of temperature dependence of resonance fields for Fe$^{3+}$ ion, there is no any phase transition at the temperature range (from -160 $^{\circ}C$ to 20 $^{\circ}C$).

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2000.07a
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• pp.548-551
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• 2000

Spinel phase LiF $e_{y}$M $n_{2-y}$ $O_4$samples are synthesized by calcining a LiOH.$H_2O$, Mn $O_2$and F $e_2$ $O_3$mixture at 80$0^{\circ}C$ for 36h in air. Preparing LiF $e_{y}$M $n_{2-y}$ $O_4$showed spinel phase with cubic phase. The ununiform distortion of the crystallite of the spinel LiF $e_{y}$M $n_{2-y}$ $O_4$was more stable than that of the pure. The discharge capacity of the cathode for the Li/LiF $e_{0.1}$M $n_{1.9}$ $O_4$cell at the first than that of the pure. The discharge capacity of the cathode for the Li/LiF $e_{0.1}$M $n_{1.9}$ $O_4$cell at the first cycle and at the 70th cycle was about 113 and 90mAh/g, respectively. This cell capacity was retained about 82% of the first cycle after 70th cycle. Impedance profile of this cell was more stable than that pure. The resistance, the capacitance and chemical diffusion coefficients of lithium ion showed approximately 80$\Omega$, 36133.87$\mu$F ; 1.4$\times$10$^{-8}$ c $m^2$ $s^{-1}$ , respectively. , respectively.ely.

• Korean Journal of Materials Research
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• v.9 no.10
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• pp.985-991
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• 1999

Corrosion behaviors of Incoloy 800H, KSA(Kaeri Superalloy)-6, Inconel 600 and Hastelloy C-276 in molten salts were investigated in the temperature range of 650 ~ $850^{\circ}C$. Due to $\textrm{Li}_{2}\textrm{O}$-induced basic fluxing mechanism, the corrosion rates of the alloys in mixed molten salt of LiC1-$\textrm{Li}_{2}\textrm{O}$ were significantly higher than those in molten salt of LiCl. In the mixed molten salt, Fe-base alloys showed higher corrosion resistance than the Ni-base alloys. and Hastelloy C-276 with high Mo and W contents exhibited the highest corrosion rate among the examined alloys. The single layer of $\textrm{LiCrO}_{2}$ was formed in molten salt of LiCl and two phase structure of a scale consisted of oxides and Ni was formed in the mixed molten salt.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.7 no.1
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• pp.6-17
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• 1997

Lithium niobate single crystals with various [Li]/[Nb] ratios were grown by the Czochralski method from melts having compositions varing between 48.6 ~ 58.0 mol % $Li_2O$. A vapor transport equilibration technique has been used to improve the homogeneity and adjust the [Li]/[Nb] ratio in small $LiNbO_3$ single crystals grown by the Czochralski method. When equilibrated with a Li-rich powder (65 mol%$Li_2O$), containing a mixture of $LiNbO_3$ and $Li_3NbO_4$, crystals of nearly stoichiometric composition can be obtained. This was established by studying the composition dependence of the following properties; lineshape, intensity and linewidth for the electron paramagnetic resonance (EPR) of $Fe^{3+}$ energy of the fundamental absorption edge and $OH^-$ absorption spectra.