• Journal of the Korean Ceramic Society
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• v.37 no.5
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• pp.466-472
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• 2000

As cathode materials of LiMn2O4-based lithium-ion secondary batteries, Li(Mn1-$\delta$M$\delta$)2O4 (M=Ni and Co, $\delta$=0, 0.05, 0.1 and 0.2) materials which Co and Ni are substituted for Mn, were syntehsized by the solid state reaction at 80$0^{\circ}C$ for 48 hours. No second phases were formed in Li(Mn1-$\delta$M$\delta$)2O4 system with substitution of Co. However, substitution of Ni caued to form a second phase of NiO when its composition exceeded over 0.2 of $\delta$ in Li(Mn1-$\delta$M$\delta$)2O4. As the results of charging-discharging test, the maximum capacity of Li(Mn1-$\delta$M$\delta$)2O4 appeared in $\delta$=0.1 for both Co and Ni. Also, Li(Mn1-$\delta$M$\delta$)2O4 electrode showed higher capacity and better cycle performance than LiMn2O4.

• Applied Chemistry for Engineering
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• v.9 no.2
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• pp.220-225
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• 1998

The spinel structured $LiMn_2O_4$ was prepared from $Li_2CO_3$ and $MnO_2$ by calcination at various temperatures in the range of $750{\sim}900^{\circ}C$. It was found that the most suitable cubic structure of $LiMn_2O_4$ was obtained by heating at $850^{\circ}C$ for 12 hrs. However, in the calcination at $900^{\circ}C$, $Mn^{4+}$ of 0.06M was changed to $Mn^{+3}$ by the oxygen loss, so that it has been shown that the formula has changed to $LiMn_2O_{3.97}$. This phenomena were in agreement with the Jahn-Teller distortion by the increment of $Mn^{+3}$ ion on the octahedral sites of the spinel structured $LiMn_2O_4$. The results showed that after 15 charge/discharge cycles in the voltage range from 3.5V to 4.3V versus Li/$Li^+$ with a current density of $0.25mA/cm^2$, the spinel structured $LiMn_2O_4$ that was prepared at $900^{\circ}C$ showed a lower discharge capacity, 82~50 mAh/g, while the $LiMn_2O_4$, prepared at $850^{\circ}C$, showed the discharge capacity of 102~64 mAh/g.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.14 no.4
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• pp.309-315
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• 2001

Crystallized $LiMn_{2-y}Mg_{y}O_4$ powder was prepared by calcing the mixture of LiOH.$H_2O$, $MnO_2$ and MgO at $800^{\circ}C$ for 36h in an air atmosphere. The structure of $LiMn_{2-y}Mg_{y}O_4$ crystallites was analyzed from powder X-ray diffraction data as a cubic spinel, space group Fd3m. Though all cathode material showed spinel phase based on cubic phase in X-ray diffraction, other peaks gradually exhibited and became intense with increasing y value in $LiMn_{2-y}Mg_{y}O_4$. However, ununiform which calculated by (111) face and (222) face was constant in spite of the increase of y value, except pure $LiMn_2O_4$. AC impedance of Li/$LiMn_{2-y}Mg_{y}O_4$ cells revealed the similar resistance of about $70\Omega$ before cycling. In addition, The impedance of Li/$LiMn_{1.9}Mg_{0.1}O_4$ cell changed during charge and discharge or after cycling.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2001.05a
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• pp.23-26
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• 2001

The properties of $LiMnO_2$ was studied as a cathode active material for lithium polymer batteries. $LiMnO_2$ cathode active materials were synthesized by the reaction of $LiOH{\cdot}H_2O$ and $Mn_2O_3$ at various temperature under argon atmosphere. The powders were characterized by the X -ray diffraction. For lithium polymer battery applications, the $LiMnO_2$ cell was characterized electrochemically by charge-discharge experiments and a.c. impedance spectroscopy. And the relationship between the characteristics of powders and electrochemical properties was studied in this research. A maximum discharge capacity of 160~170 mAh/g for o-$LiMnO_2$ cell was achieved. The capacity of o-$LiMnO_2$ electrode demonstrated better than of the spinel $LiMnO_2$ by solid-state reaction.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.25 no.5
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• pp.398-402
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• 2012

Synthesis of $Li_2MnSiO_4$ was attempted by the conventional solid-state reaction method, and the phase formation behavior according to the change of the calcination condition was investigated. When the mixture of the three source materials, $Li_2O$, MnO and $SiO_2$ powders, were used for calcination in air, it was difficult to develop the $Li_2MnSiO_4$ phase because the oxidation number of $Mn^{2+}$ could not be maintained. Therefore, two-step calcination was applied: $Li_2SiO_3$ was made from $Li_2O$ and $SiO_2$ at the first step, and $Li_2MnSiO_4$ was synthesized from $Li_2SiO_3$ and MnO at the second step. It was easy to make $Li_2MnSiO_3$ from $Li_2O$ and $SiO_2$. $Li_2MnSiO_4$ single phase was developed by the calcination at $900^{\circ}C$ for 24 hr in Ar atmosphere as the oxidation of $Mn^{2+}$ was prevented. However, the $Li_2MnSiO_4$ was ${\gamma}-Li_2MnSiO_4$, one of the polymorph of $Li_2MnSiO_4$, which could not be used as the cathode materials in Li-ion batteries. By applying the additional low temperature annealing at $400^{\circ}C$, the single phase ${\beta}-Li_2MnSiO_4$ powder was synthesized successfully through the phase transition from ${\gamma}$ to ${\beta}$ phase.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2008.11a
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• pp.277-278
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• 2008

Orthorhombic $LiMnO_2$(o-$LiMnO_2$) has attracted public attentions as a cathode materials of Lithium ion battery because it has low cost and high theoretical discharge capacity of 285mAh $g^{-1}$. In our study, o-$LiMnO_2$ is synthesized by quenching method. To verify their phase structure, X-ray diffraction is accomplished. Test cells are assembled to check electrochemical characteristics using acquired o-$LiMnO_2$ cathode and carbon anode. Charge/Discharge cycling was carried out for 50cycles. And impedance was measured at 1, 2, 5, 10, 30, 50cycle. During cycle test, the max discharge capacity was recorded 139mAh $g^{-1}$ at 10cycle.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.6 no.4
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• pp.600-608
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• 1996

Specific structural properties of Li intercalation reaction into the spinel relatedmanganese dioxide, $Li_{x}Mn_{2}O_{4}(0.2{\leq}x{\leq}2.0)$, are investigated by X-ray diffractional and electrochemical studies of Li/1M $LiClO_{4}$-propylene carbonate solution/$Li_{x}Mn_{2}O_{4}$ cell. The effect of the chemical composition and the reaction temperature on electrochemical parameter of $Li_{x}Mn_{2}O_{4}$ are studied by the phenomena of phase-transition, analysis of crystal lattice, fine structure, and thermal analysis. Treatment of the spinel $Li_{x}Mn_{2}O_{4}$ with aqueous acid was found to result in conversiton of $Li_{x}Mn_{2}O_{4}$ to nearly pure $MnO_{2}$, as evidenced by a reduction in the lattice constant $a_{c}$ from 8.255 to $8.031\;{\AA}$. At a composition range of $0.2{\leq}x{\leq}0.6$ in $Li_{x}Mn_{2}O_{4}$ the reduction proceeded in a homogeneous phase, which was characterized by a constant voltage of 3.9~3.7 V together with a lattice constant of $8.255\;{\AA}$.

• Journal of the Korean Ceramic Society
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• v.35 no.9
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• pp.995-1001
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• 1998

As a basic study for cathode materials of {{{{ { {LiMn }_{2 }O }_{4 } }}-based lithium-ion secondary batteries Li({{{{ { { { {Mn }_{1-$\delta$ }Nb }_{$\delta$} )}_{2 }O }_{4 } }} ($\delta$=0.05, 0.1, 0.2) materials which Nb is substituted for Mn were synthesized by the solid state reaction at 80$0^{\circ}C$ and 110$0^{\circ}C$ respectively. The second phase {{{{ { LiNbO}_{3 } }} appeared above $\delta$=0.1 As the result of im-pedance analysis as the amount of substituted Nb increased the resistivity of grain boundary increased greatly. Compared to undoped-{{{{ { {LiMn }_{2 }O }_{4 } }} the electrical conductivity of Li({{{{ { { { {Mn }_{1-$\delta$ }Nb }_{$\delta$} )}_{2 }O }_{4 } }} decreased slightly but is charging capacity and potential plateau increased.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2005.07a
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• pp.418-419
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• 2005

$\o-LiMnO_2$ is known to have poor cycle performance causing the irreversible phase transformation on cycling. In this paper, the effect of chemical substitution on improving cycle performance of $o-LiMnO_2$ was studied at the compositions of $LiCr_xMn_{1-x}O_2$(x=0, 0.1, 0.2, 0.4). XRD is showed that structure of $LiCr_xMn_{1-x}O_2$ transformed from orthorhombic to spinel according to the increase of substitute degree. For lithium ion battery applications, $LiCr_xMn_{1-x}O_2$/Li cell were characterized electrochemically by charge/discharge cycling.

• Korean Chemical Engineering Research
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• v.49 no.5
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• pp.541-547
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• 2011

Nanorod-clustered $MnO_2$ precursors with ${\alpha}$-, ${\beta}$-, and ${\gamma}$-phases are synthesized by hydrothermal reaction of $MnSO_45H_2O$ and $(NH_4)S_2O_8$. The formation of nanorod-clustered ${\beta}-MnO_2$ is particularly confirmed under the conditions of high reactant concentration and hydrothermal reaction at $150^{\circ}C$. The spinel $LiMn_2O_4$ nanorod-clusters are also prepared by lithiating the $MnO_2$ precursors, varying the concentration of lithiating agent ($LiC_3H_3O_2{\cdot}2H_2O$) and heat treatment temperature, and characterized for use as cathode material of lithium-ion batteries. As a result, the nanorod-clustered $LiMn_2O_4$ prepared from the ${\beta}-MnO_2$ at higher $LiC_3H_3O_2{\cdot}2H_2O$ concentration and the annealing at $800^{\circ}C$ is proven to show the cubic spinel structure and to achieve the high initial discharge capacity of 120 mAh/g.