• 한국세라믹학회지
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• 제36권7호
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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.

• 한국결정성장학회지
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• 제10권3호
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• pp.239-244
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• 2000

$LiMn_2$$O_4$Spine에 Li 과량 및 Mn 대신 Co를 일부 치환시킨 $_{1+x}$ Co$_{y}$ Mn$_{2-y}$ $O_4$(0$\leq$x$\leq$0.2,y=0,1/9,1/6) spinel에 대한 합성온도 결정, 상의 생성 등 고온 상평형에 대해 연구하였다. 고온 합성에 따른 제 2상의 생성을 방지하기 위해 저온합성이 가능한 습식화학적 합성법중 하나인 oxalate 침전법을 사용하여 $600^{\circ}C$ 이하에서 단일상의 spinel로 합성하였다. 이렇게 합성된 분말에 대해 TG-DTA분석 및 고온에서 급냉한 분말에 대한 XRD분석을 통해 질량(산소)의 증감에 연관된 가역적인 상전이 온도인 $T_1$, $T_2$및 $T_{2'}$ 들을 확인하였으며, 첨가된 Li의 양과 치환된 Co의 양에 따른 격자상수, 상전이 온도의 변화, 고온상의 안정성 등에 대해 연구하였다. 본 연구를 통해 Li$_{1+x}$ Co$_{y}$ Mn$_{2-y}$ $O_4$spinel의 합성온도 및 냉각속도 둥 합성과정 결정에 필요한 결과들을 얻을 수 있었다.

• 한국세라믹학회지
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• 제37권6호
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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$0^{\circ}C$.

• 한국재료학회:학술대회논문집
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• 한국재료학회 1996년도 재료학회 춘계학술발표회
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• pp.149-149
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• 1996

• 대한전기학회:학술대회논문집
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• 대한전기학회 1997년도 하계학술대회 논문집 C
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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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• 제4권1호
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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.

• 한국세라믹학회지
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• 제36권9호
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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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• 제18권11호
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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.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2002년도 하계학술대회 논문집 Vol.3 No.2
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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 Electrochemical Science and Technology
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• 제13권1호
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• pp.128-137
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• 2022

For this study, the sol gel method was used to synthesize the spinel LiNi_0.5Mn_1.5O₄ (LNMO) electrode material. Structural, morphological, electrochemical, and kinetic aspects of the LNMO have been characterized. The synthesized LNMO was indexed with the Fd3m cubic space group. The excellent capacity retention indicates that the spinel framework of LNMO has the ability to withstand high rate charge-discharge throughout long cycle tests. The Li diffusion coefficient (D_Li) changes non-monotonically across three orders of magnitude, from 10^-9 to 10^-12 cm² s^-1 determined from GITT method. The variation of D_Li seemed to be related to three oxidation reactions that happened throughout the charging process. A small dip in D_Li at the beginning stage of Li deintercalation is correlated with the oxidation of Mn³⁺ to Mn⁴⁺. While two pronounced D_Li minima at 4.7 V and 4.75 V are due to the oxidation of Ni²⁺/Ni³⁺ and Ni³⁺/Ni⁴⁺ respectively. The depletion of D_Li at the high voltage region is attributed to the occurrence of two successive phase transformation phenomena.