• Journal of Powder Materials
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• v.25 no.4
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• pp.296-301
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• 2018

In this study, an experiment is performed to recover the Li in $Li_2CO_3$ phase from the cathode active material NMC ($LiNiCoMnO_2$) in waste lithium ion batteries. Firstly, carbonation is performed to convert the LiNiO, LiCoO, and $Li_2MnO_3$ phases within the powder to $Li_2CO_3$ and NiO, CoO, and MnO. The carbonation for phase separation proceeds at a temperature range of $600^{\circ}C{\sim}800^{\circ}C$ in a $CO_2$ gas (300 cc/min) atmosphere. At $600{\sim}700^{\circ}C$, $Li_2CO_3$ and NiO, CoO, and MnO are not completely separated, while Li and other metallic compounds remain. At $800^{\circ}C$, we can confirm that LiNiO, LiCoO, and $Li_2MnO_3$ phases are separated into $Li_2CO_3$ and NiO, CoO, and MnO phases. After completing the phase separation, by using the solubility difference of $Li_2CO_3$ and NiO, CoO, and MnO, we set the ratio of solution (distilled water) to powder after carbonation as 30:1. Subsequently, water leaching is carried out. Then, the $Li_2CO_3$ within the solution melts and concentrates, while NiO, MnO, and CoO phases remain after filtering. Thus, $Li_2CO_3$ can be recovered.

• Applied Chemistry for Engineering
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• v.17 no.3
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• pp.250-254
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• 2006

Reaction of $CO_2$ with $Li_{2}ZrO_{3}$ has been investigated in a TGA and the effects of $H_{2}$ and CO on the removal of $CO_{2}$ using $Li_{2}ZrO_{3}$ were evaluated in a packed bed reactor. The initial rate of $CO_{2}$ removal reaction of $Li_{2}ZrO_{3}$ increased with the increase of gas flow rate up to 100 mL/min and then was maintained, which implied the disappearance of the gas film resistance. The reaction of $CO_{2}$ with $Li_{2}ZrO_{3}$ took place as the first order and the range of optimum temperature was found to be about $500{\sim}600^{\circ}C$. XRD and SEM analysis showed the formation of crystalline $Li_{2}ZrO_{3}$ and porous $Li_{2}ZrO_{3}$/$ZrO_{2}$. The presence of $H_{2}$ did not affect the adsorption of $CO_2$ with $Li_2ZrO_3$. On the other hand, CO inhibited the sorption of $CO_{2}$ into $Li_{2}CO_{3}$(L) on $Li_{2}ZrO_{3}$.

• Proceedings of the Korean Vacuum Society Conference
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• 2011.02a
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• pp.183-183
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• 2011

리튬 이온 배터리의 cathode 및 electrolyte 재료로 사용되는 LiCoO2을 sputtering이나 pulsed laser deposition을 이용하여 박막으로 증착하기 위해서는 target이 필요하다. Target은 원료 분말을 가압 성형한 후 고온에서 소결하여 제조된다. LiCoO2 target 제조과정에서 고밀도를 얻기 힘들고 Li 성분의 증발이 일어난다. 또한 Li2O 분말은 흡습성이 매우 크다. 본 연구에서는 시간과 온도를 조절하여 최적화된 소결 과정을 통해 target의 밀도가 이론밀도와 근사한 값을 갖도록 하고, LiCoO2 또는 Co3O4 분말에 각각 흡습성이 낮은 Li2CO3 분말을 첨가하여 Li 성분을 조절하였다. Li과 Co의 조성비가 1:1-2:1인 고밀도의 LiCoO2 target을 제조하여 박막 증착 후 Li과 Co의 조성비가 1:1이 되도록 하였다.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2005.07a
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• pp.318-319
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• 2005

본 연구에서는 $LiCoO_2/LiNi_{1/3}Mn_{1/3}Co_{1/3}O_2$ 혼합 정극활물질로 사용하여 전극을 제작하고 성능을 평가하였다. $LiCoO_2/LiNi_{1/3}Mn_{1/3}Co_{1/3}O_2$와 $LiCoO_2$의 혼합비에 따른 충방전 거동 및 임피던스 변화를 측정하였다. 각 조성에서의 초기용량은 160 ~ 170 mAh/g 정도였으며, $LiNi_{1/3}Mn_{1/3}Co_{1/3}O_2$의 첨가 비율이 증가함에 따라 비용량이 증가하였으나 고율에서의 방전용량은 낮았다.

• Archives of Metallurgy and Materials
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• v.64 no.2
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• pp.481-485
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• 2019

This study was attempted to study for recovery of Li as Li₂CO₃ from cathode active material, especially NCA (LiNiCoAlO₂), recovered from spent lithium ion batteries. This consists of two major processes, carbonation using CO₂ and water leaching. Carbonation using CO₂ was performed at 600℃, 700℃ and 800℃, and NCA (LiNiCoAlO₂) was phase-separated into Li₂CO₃, NiO and CoO. The water leaching process using the differences in solubility was performed to obtain the optimum conditions by using the washing time and the ratio of the sample to the distilled water as variables. As a result, NCA (LiNiCoAlO₂) was phase-separated into Li₂CO₃ and NiO, CoO at 700℃, and Li₂CO₃ in water was recovered through vacuum filtration after 1 hour at a 1:30 weight ratio of the powder and distilled water. Finally, Li₂CO₃ containing Li of more than 98 wt.% was recovered.

• Resources Recycling
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• v.9 no.4
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• pp.37-43
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• 2000

Leaching of $LiCoO_2$ as a cathodic active materials for recovering Li and Co from spent lithium ion battery was investigated in terms of reaction variables. At the optimum condition determined in the previous work, Li and Co in a $H_2SO_4$ and $HNO_3$ solution were dissolved 70~80% and 40%, respectively. Li and Co were leached over 95% with the addition of a reductant such as $Na_2S_2O_3$ or $H_2O_2$. This behavior is probably due to the reduction of $Co^{3+}$ to $Co^{2+}$. Leaching of $LiCoCo_2$ powder obtained by calcination of an electrode materials from spent batteries was also carried out. Leaching efficiency of Li and Co were over 99% at the optimum condition with $H_2O_2$ addition of 1.7 vol.%. It seems to be due to the activation of $LiCoO_2$ by repeated charging and discharging or an imperfect crystal structure by deintercalation of Li.

• Korean Chemical Engineering Research
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• v.44 no.5
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• pp.535-539
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• 2006

Effects of alkaline additives on the $CO_2$ removal reaction have been investigated by a thermogravimetric analyzer. $Li_2ZrO_3$ was synthesized by soild reaction of $ZrO_2$ with $Li_2CO_3$ and then alkali chemicals were added to the synthesized $Li_2ZrO_3$ and then heat treatment was carried out. Addition of alkali chemicals enhanced the reactivity of $Li_2ZrO_3$ with the following order; $K_2CO_3>NaCl>LiCl>Na_2CO_3$, which were resulted from the formation of partially melted $Li_2CO_3$. SEM photographs showed the presence of melted state and the XRD results showed that the chemical states of added salts were not changed. Addition of NaCl caused the induction time of about 60 min at the initial reaction stage and the addition of $Na_2CO_3$ inhibited the decomposition of $Li_2CO_3$ at about $700{\sim}750^{\circ}C$.

• Electrical & Electronic Materials
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• v.7 no.4
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• pp.317-324
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• 1994

In this study, new preparation method of LiCoO$_{2}$ was applied to develop cathode active material for Li rechargeable cell, and followed by X-ray diffraction analysis, electrochemical properties and initial charge/discharge characteristics as function of current density. HC8A72- and CC9A24-LiCoO$_{2}$ were prepared by heating treatment of the mixture of LiOH H$_{2}$O/CoCO$_{3}$(1:1 mole ratio) and the mixture of Li$_{2}$CO$_{3}$/CoCO$_{3}$(1:2 mole ratio) at 850 and 900.deg. C, respectively. Two prepared LiCoO$_{2}$s were identified as same structure by X-ray diffraction analysis. a and c lattice constant were 2.816.angs. and 14.046.angs., respectively. The electrochemical potential of CFM-LiCoO$_{2}$(Cyprus Foote Mineral Co.'s product), HC8A72-LiCoO$_{2}$ and CC9A24 LiCoO$_{2}$ electrode were approximately between 3.32V and 3.42V vs. Li/Li reference electrode. Stable cycling behavior was obtained during the cyclic voltammetry of LiCoO$_{2}$ electrode. According as scan rate increases, cathodic capacity decreases, but redox coulombic efficiency was about 100% at potential range between 3.6V and 4.2V vs. Li/Li reference electrode. Cathodic capacity of HC8A72-LiCoO$_{2}$ was 32% higher than that of CFM-LiCoO$_{2}$ and that of CC9A24-LiCoO$_{2}$ was 47% lower than that of CFM-LiCoO$_{2}$ at 130th cycle in the condition of lmV/sec scan rate. Constant cur-rent charge/discharge characteristics of LiCoO$_{2}$/Li cell showed increasing Ah efficiency with initial charge/discharge cycle. Specific discharge capacities of CFM and HC8A72-LiCoO$_{2}$ cathode active materials were about 93mAh/g correspondent to 34% of theretical value, 110mAh/g correspondent to 40% of theretical value, respectively. In the view of reversibility, HC8A72-LiCoO$_{2}$ was also more excellent than CFM- and CC9A24-LiCoO$_{2}$.

• Journal of the Korean Ceramic Society
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• v.37 no.8
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• pp.817-823
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• 2000

A solid-state electrochemicall cell for sensing CO2 gas was fabricated using a solid electrolyte of Li2CO3-Li3PO4-Al2O3 mixture and a reference electrode of LiMn2O4. The e.m.f. (electromotive force) of sensor showed a good accordance with theoretical Nernst slope (n=2) for CO2 gas concentration range of 100-10000 ppm above 35$0^{\circ}C$. The e.m.f. of sensor was constant regardless of oxygen partial pressure at the high temperature above 0.1 atm. It was, however, a little depended on oxygen partial pressure as the pressure decreased below 0.1 atm. The oxygen-dependency of our sensor gradually disappeared as the operating temperature increased. The sensing behavior of our CO2 sensor was affected by the presence of water vapor, but its effect was small comparing with other sensors.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.11 no.4
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• pp.154-159
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• 2001

(Li,Al)$MnO_2(OH)_2$:Co compound was synthesized by hydrothermal method. $MnO_2$, LiOH.$H_2$O, $Co_3O_4$ and $Al(OH)_3$ were used as starting materials and the optimum conditions for synthesis of monolithic (Li,Al)$MnO_2(OH)_2$:Co compound were as follows : reaction temperature; $200^{\circ}C$, reaction time; 3 days, hydrothermal solvent; 3M-KOH solution, reaction apparatus; seesaw type, atomic ratio of Li:Al:Mn;Co = 1:2.1:2.5~2:0.5~1. Monolithic(Li,Al)$MnO_2(HO)_2$:Co compound synthesized in this work had a god crystallinity and excellent color forming effect as a blue pigment compatible with natural mineral. The particles of the synthesized (Li,Al)$MnO_2(OH)_2$:Co compound have hexagonal plate shape with the size of 0.5~1 $\mu\textrm{m}$.