• Journal of the Korean Ceramic Society
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• v.38 no.4
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• pp.307-307
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• 2001

Combustion process with citrate was used to produce the LiMn$_2$O$_4$powder. Precursors are pre-ignited in open air followed by post-heating in the range from $600^{\circ}C$ to 80$0^{\circ}C$ for 4h. With varying the molar ratio (R) of ethylene glycol (EG) to citric acid (CA) from 0 to 4, the effect of EG content on powder characteristics is evaluated. Vacuum drying promote the auto-ignition at room temperature. With small addition of EG metal ion was selectively segregated with organic substances and undesired lithium evaporation occurred during post-heating. LiMn$_2$O$_4$phase which is produced by combustion reaction was decomposed back to Mn$_3$O$_4$because the reaction temperature was higher than 95$0^{\circ}C$. With increasing EG content, the homogeneity of LiMn$_2$O$_4$powder increased and specific surface area increased. And lithium evaporation during vacuum drying and/or ignition also increased.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.22 no.4
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• pp.194-199
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• 2012

The $LiMn_{1.5}Ni_{0.5}O_4$, substituting a part of Mn with Ni in the $LiMn_2O_4$, the spinel structure has good charge-discharge cycle stability and high discharge capacity at 4.7 V. In this study $LiMn_{1.5}Ni_{0.5}O_4$ powders were synthesized by polymerization complex method. The effect on the characteristics of synthesized $LiMn_{1.5}Ni_{0.5}O_4$ powders was studied with citric acid (CA) : metal ion (ME) molar ratio (5 : 1, 10 : 1, 15 : 1, 30 : 1) and calcination temperature ($500{\sim}900^{\circ}C$). Single phase of $LiMn_{1.5}Ni_{0.5}O_4$ was observed from XRD analysis on the powders calcined at low ($500^{\circ}C$) and high temperatures ($900^{\circ}C$). The crystalline size and crystallinity increased with calcination temperature. At low calcination temperature the particle size decreased and specific surface area increased as the CA molar ratio increased. On the other hand, high particle growth rate at high calcination temperature interfered the particle size reduction and specific surface area increase induced by the increase of CA molar ratio.

• Bulletin of the Korean Chemical Society
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• v.34 no.2
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• pp.622-628
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• 2013

Nanocrystalline spinel lithium manganese oxide ($LiMn_2O_4$) powders with narrow-size-distribution, pure-phase particles, and high crystallinity with an average crystallite size of about 70 nm were synthesized at $600^{\circ}C$ for 6 h in air by freeze drying method. Spinel $LiMn_2O_4$ is also prepared by sol-gel using citric acid as a chelating agent. The influence of different parameters such as pH conditions, solvent, molar ratio of citric acid to total metal ions, calcination temperature, starting material on the structure, morphology and purity of this oxide was investigated. The results of sol-gel method show that pure $LiMn_2O_4$ with average crystallite size of about 130 nm can be produced from nitrate salts as starting materials at $800^{\circ}C$ for 6 h in air. The optimum pH and molar ratio of chelating agent to total metal ions are $4{\leq}pH{\leq}6$ and 1.0, respectively. A possible mechanism on the formation of the nanocrystallines synthesized by sol-gel was also discussed. At the end a comparison of the differences between two methods was made on the basis of x-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA) tests.

• Korean Chemical Engineering Research
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• v.47 no.1
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• pp.84-88
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• 2009

Al doped $LiMn_2O_4$ cathode powders with fine size were synthesized by an ultrasonic spray pyrolysis method from the spray solution with citric acid and ethylene glycol. The as-prepared powders with spherical shape, porous structure and micron size turned into $LiMn_{11/6}Al_{1/6}O_4$ powders with micron size and regular morphology after post-treatment above $800^{\circ}C$. The $LiMn_{11/6}Al_{1/6}O_4$ powders had low initial discharge capacity of 94 mAh/g at a post-treatment temperature of $700^{\circ}C$. As the post-temperature increased from $750^{\circ}C$ to $1,000^{\circ}C$, the initial discharge capacities of the $LiMn_{11/6}Al_{1/6}O_4$ powders changed from 103 to 117 mAh/g. The $LiMn_{11/6}Al_{1/6}O_4$ powders had the maximum discharge capacity at a post-treatment temperature of $750^{\circ}C$. However, the $LiMn_{11/6}Al_{1/6}O_4$ powders post-treated at a temperature of $900^{\circ}C$ had the good cycle properties. The discharge capacities of the $LiMn_{11/6}Al_{1/6}O_4$ powders dropped from 107 to 100 mAh/g (93% capacity retention) by the 70th cycle at a current density of 0.1 C.