• Journal of the Korean Ceramic Society
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• v.36 no.7
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• pp.698-704
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• 1999

Li rich Li1+xMn2-xO4(x=0.07) spinel powders were prepared by an oxalate precipitation of wet chemical methods at temperature lower than $600^{\circ}C$. The FTIR results showed that the powders prepared at $600^{\circ}C$ had high degree of crystal quality comparing with the spinel powders prepared by solid state reaction at 75$0^{\circ}C$ which was the lowest synthesis temperature of the solid state reaction method. The particle size of powders prepared by the oxalate precipitation at $600^{\circ}C$ was smaller than 0.2${\mu}{\textrm}{m}$ and the specific surface area was 11.01 m2/g A heat treatment over 90$0^{\circ}C$ formed second phase in the precipitates. It was shown that there were phase transitions at temperatures. T1,T2 and T2. The transitions involved weight loss and gain during heating and cooling. The low temperature synthesis below $600^{\circ}C$ avoided the second phase formation and the prepared powders showed improved compositional and physical properties for secondary lithium battery applications.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.10 no.3
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• pp.239-244
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• 2000

Synthesis and high temperature phase stability of $_{1+x}$ Co$_{y}$ Mn$_{2-y}$ $O_4$(0$\leq$x$\leq$0.2,y=0,1/9,1/6) spinel, both the excess lithium and cobalt added, have been studied. The spinel was prepared by oxalate precipitation method as the wet chemical process. Oxalate derived spinel was synthesized by heating of precipitates at temperature lower than $600^{\circ}C$. As a result of the TG-DTA and XRD analysis of prepared and quenched powders, it was found that reversible phase transitions started at temperatures $T_1$, $T_2$및 $T_{2'}$. The transitions involved weight (oxygen) loss and gain during heating and cooling. The effects of Li excess and Co doping on the spinel lattice constant, phase stability and transition temperatures of the prepared powders are investigated. This study would provide important data for determining the spinel preparation process such as synthesis temperature and cooling speed.

• Journal of the Korean Ceramic Society
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• v.37 no.6
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• pp.564-568
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• 2000

Spinel LiMn2O4 catalyst with submicron and single phase particles was synthesized at 48$0^{\circ}C$ for 12 hr in air by a sol-gel method. The spinel LiMn2O4 was deoxidized by hydrogen at various temperatures. Effects of physiochemical properties of the catalyst reduced by hydrogen were examined with X-ray diffractometer, thermogravimetric analysis and scanning electron microscope. The decomposition rate of carbon dioxide was measrued using the catalyst deosidized at 35$0^{\circ}C$.

• Proceedings of the Materials Research Society of Korea Conference
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• 1996.05a
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• pp.149-149
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• 1996

• Proceedings of the KIEE Conference
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• 1997.07d
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• pp.1462-1464
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• 1997

The spinel $LiMn_2O_4$ has been synthesized by solid-state reaction. $LiMn_2O_4$ which includes 3 mix $Li_2CO_3$ or $LiNO_3$ and $MnO_2$ prepared by Prelim heating at $350^{\circ}C$ for 24hr. $LiMn_2O_4$ fired at temp range from $600^{\circ}C$ to $800^{\circ}C$ for 48hr. The structure a electrochemical characteristics of spinel $LiMn_2O_2$ wh fabricated by changing sintering condition from st materials are investigated. The spinel $LiMn_2O_4$ prepared by the mixture of L CMD at $800^{\circ}C$ for 48hr showed an initial charge ca of 146mAh/g. The spinel $LiMn_2O_4$ prepared by the m of $LiNO_3$/CMD at $600{\sim}800^{\circ}C$ for 48hr stabilized ch discharge capacity after 50th cycles.

• Journal of Electrochemical Science and Technology
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• v.4 no.1
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• pp.34-40
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• 2013

The structural and electrochemical properties of $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ ($Fd{\bar{3}}m$, disordered spinel) cathode material were studied and compared with stoichiometric $LiNi_{0.5}Mn_{1.5}O_4$ ($P4_332$, ordered spinel). First cycle discharge capacity of $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ was similar to that of $LiNi_{0.5}Mn_{1.5}O_4$ at C/3 and 1C rate, but cycling performance of $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ was better than that of $LiNi_{0.5}Mn_{1.5}O_4$ especially at high rate of 1C. This can be explained by performing synchrotron based in-situ XRD and results of GITT measurements. It is considered that faster lithium ion diffusion in the $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ cathode results in the improvement of the rate capability. To study structural changes during cycling, synchrotron in-situ XRD patterns of both the samples were recorded at C/3 and 1C rate. Compared to stoichiometric $LiNi_{0.5}Mn_{1.5}O_4$, disordered $Li_{0.99}Ni_{0.46}Mn_{1.56}O_4$ spinel sample has pseudo one phase behavior and one step phase transition between two cubic phases. So, $LiNi_{0.5}Mn_{1.5}O_4$ would experience a much greater strain and stress, originating from the two phase transitions between three cubic phases and suffer from capacity loss during cycling especially at high rate.

• Journal of the Korean Ceramic Society
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• v.36 no.9
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• pp.930-936
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• 1999

For LiMn2O4 based spinel structures the stoichiometric reaction conditions need be considered carefully because the electrical properties depend on the structural stability. In order to obtain the homogeneous compound the Pechini process was chosen which could obtain a stoichiometry phase even low temperature and dependency of the synthetic condition on structural stability and electrochemical performance was investigated. X-ray diffraction studies showed that the compounds doped with transition metal have smaller lattice constants than those un doped. The dc conductivity was evaluated by a four probe method in the low and high temperature region respectively. The variations of basal spacings for the cathode were detected to be dependent on the extent of current flows (under dc)

• Bulletin of the Korean Chemical Society
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• v.18 no.11
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• pp.1153-1158
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• 1997

The powder characteristics of LiMn2O4 prepared by the citrate sol-gel method have been investigated. The optimum pH for the preparation of homogeneous citrate gel was calculated by the theoretical consideration of thermodynamic equilibrium constants for metal-citrate complexes and metal salts. The obtained citrate gel was prefired at 300 ℃ and calcined at 300-700 ℃ for 1 h. The obtained powders were characterized by TG/DSC, FT-IR spectrometer, X-ray diffractometer, SQUID magnetometer, SEM, and particle size analyzer. It was observed that the mixed phases of spinel LiMn2O4 and Mn3O4 were transformed into spinel LiMn2O4 phase and the vibrational bands due to the carbonate and nitrate were also disappeared over 400 ℃. At temperatures below 150 K, inverse molar susceptibilities of every sample began to show an antiferromagnetic ordering of Mn magnetic moments.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2002.07b
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• pp.707-710
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• 2002

Spinel $LiMn_2O_4$ and $LiMn_{1.9}Mg_{0.05}Zn_{0.05}O_4$ powders were synthesized by solid-state method at $800^{\circ}C$ for 36h. Crystal structure and electrochemical properties were analyzed by X-ray diffraction, charge-discharge test, cyclic voltammetry and ac impedance to $LiMn_2O_4$ and $LiMn_{1.9}Mg_{0.05}Zn_{0.05}O_4/Li$. All cathode material showed spinel structure in X-ray diffraction. $LiMn_{1.9}Mg_{0.05}Zn_{0.05}O_4/Li$ cell substituted $Mg^{2+}$ and $Zn^{2+}$ showed excellent discharge capacities than other cells, which it presented about 120mAh/g at the 1st cycle and about 73mAh/g at the 250th cycle, respectively. AC impedance of $LiMn_{1.9}Mg_{0.05}Zn_{0.05}O_4/Li$ cells showed the similar resistance of about $65{\sim}110{\Omega}$ before cycling.

• Journal of the Korean Ceramic Society
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• v.47 no.6
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• pp.633-637
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• 2010

In this study, lithium manganese oxide spinel ($LiMn_{1.9}Fe_{0.1}Nb_{0.0005}O_4$) as a cathode material of lithium ion secondary batteries is synthesized with spray drying, and in order to increase its crystallinity and electrochemical properties, the granulated $LiMn_{1.9}Fe_{0.1}Nb_{0.0005}O_4$ particle surface is coated with lithium titanium oxide spinel ($Li_4Ti_5O_{12}$) through a sol-gel method. The granulated particles present a higher tap density and lower specific surface area. The crystallinity and discharge capacity of the $Li_4Ti_5O_{12}$ coated material is relatively higher than uncoated material. With the coating layer, the discharge capacity and cycling stability are increased and the capacity fading is suppressed successfully.