• 한국전기화학회:학술대회논문집
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• 2002.07a
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• pp.117-122
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• 2002

고체산화물 연료전지의 구성요소인 양극(공기극)을 GNP와 Pechini 법을 이용하여 $(La{1-x}Sr_x)MnO_3$ 양극을 합성하여 합성한 분말의 특성과 단위전지로 사용하기 위한 조건에서의 특성을 측정하였다. GNP로 합성한 분말의 경우 직접 $(LaSr)MnO_3$ 단일 결정상을 얻을 수 있었으나, Pechini 법으로 합성한 분말의 경우는 비정질이었다. 또한 각각의 방법으로 합성한 분말의 입자형태는 구형이었고 1차상 입자크기는 GNP가 40nm, Pechini, 법으로 합성한 경우 20nm 정도의 크기를 갖고 있었다. GNP로 합성한 분말의 입자크기와 비표면적의 경우 glycine의 첨가량이 증가함에 따라 입자크기는 감소하였으나 최적 glycine 첨가량은 2.0mole 였고, 이 때 평균2차상의 입자크기는 $13.24{\mu}m$로 agglomeration 되어있었다. 최적 cathode조성은 GNP법으로 합성한 $(La_{0.9}Sr_{0.1}MnO_3$로서 가능하였고, 이 조성에서의 열팽창계수는 $9.89\times10^{-6}/^{\circ}C$이고, 전기전도도($1200^{\circ}C$에서 2시간소결)는 110 S/cm을 나타내었다.

• Resources Recycling
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• v.31 no.4
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• pp.40-48
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• 2022

In waste lithium iron phosphate (LFP) batteries, the cathode material contains approximately 4% lithium. Recycling the constituent elements of batteries is important for resource circulation and for mitigating the environmental pollution. Li contained in the waste LFP cathode powder was selectively leached using persulfate-based oxidizing agents, such as sodium persulfate, potassium persulfate, and ammonium persulfate. Leaching efficiency and waste LFP powder properties were compared and analyzed. Pulp density was used as a variable during leaching, which was performed for 3 h under each condition. The leaching efficiency was calculated using the inductively coupled plasma (ICP) analysis of the leachate. All types of persulfate-based oxidizing agents used in this study showed a Li leaching efficiency over 92%. In particular, when leaching was performed using (NH₄)₂S₂O₈, the highest Li leaching percentage of 93.3% was observed, under the conditions of 50 g/L pulp density and an oxidizing agent concentration of 1.1 molar ratio.

• Resources Recycling
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• v.33 no.3
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• pp.21-29
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• 2024

Globally, the demand for electric vehicles (EVs) is surging due to carbon-neutral strategies aimed at decarbonization. Consequently, the demand for lithium-ion batteries, which are essential components of EVs, is also rising, leading to an increase in the generation of spent batteries. This has prompted research into the recycling of spent batteries to recover valuable metals. In this study, we aimed to selectively leach and recover lithium from the cathode material of spent LFP batteries. To enhance the reaction surface area and reactivity, the binder in the cathode material powder was removed, and the material was subjected to heat treatment in both atmospheric and nitrogen environments across various temperature ranges. This was followed by a mechanochemical process for aqueous leaching. Initially, after heat treatment, the powder was converted into a soluble lithium compound using sodium persulfate (Na₂S₂O₈) in a mechanochemical reaction. Subsequently, aqueous leaching was performed using distilled water. This study confirmed the changes in the characteristics of the cathode material powder due to heat treatment. The final heat treatment in a nitrogen atmosphere resulted in a lithium leaching efficiency of approximately 100% across all temperature ranges.

• Journal of Powder Materials
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• v.31 no.2
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• pp.163-168
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• 2024

As the demand for lithium-ion batteries for electric vehicles is increasing, it is important to recover valuable metals from waste lithium-ion batteries. In this study, the effects of gas flow rate and hydrogen partial pressure on hydrogen reduction of NCM-based lithium-ion battery cathode materials were investigated. As the gas flow rate and hydrogen partial pressure increased, the weight loss rate increased significantly from the beginning of the reaction due to the reduction of NiO and CoO by hydrogen. At 700 ℃ and hydrogen partial pressure above 0.5 atm, Ni and Li₂O were produced by hydrogen reduction. From the reduction product and Li recovery rate, the hydrogen reduction of NCM-based cathode materials was significantly affected by hydrogen partial pressure. The Li compounds recovered from the solution after water leaching of the reduction products were LiOH, LiOH·H₂O, and Li₂CO₃, with about 0.02 wt% Al as an impurity.

• Clean Technology
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• v.30 no.1
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• pp.28-36
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• 2024

As demand for electric vehicles increases, the market for lithium-ion batteries is also rapidly increasing. The battery life of lithium-ion batteries is limited, so waste lithium-ion batteries are inevitably generated. Accordingly, lithium was selectively preleached from waste lithium iron phosphate (LiFePO₄, hereafter referred to as the LFP) cathode material powder among lithium ion batteries, and iron phosphate (FePO₄) powder was recovered. The recovered iron phosphate powder was mixed with alkaline sodium carbonate (Na₂CO₃) powder and heat treated to confirm its crystalline phase. The heat treatment temperature was set as a variable, and then the leaching rate and powder characteristics of each ingredient were compared after water leaching using Di-water. In this study, lithium showed a leaching rate of approximately 100%, and in the case of powder heat-treated at 800 ℃, phosphorus was leached by approximately 99%, and the leaching residue was confirmed to be a single crystal phase of Fe₂O₃. Therefore, in this study, lithium, phosphorus, and iron components were individually separated and recovered from waste LFP powder.

• Journal of Powder Materials
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• v.21 no.2
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• pp.131-136
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• 2014

Cathode materials and their precursors are prepared with transition metal solutions recycled from the the waste lithium-ion batteries containing NCM (nickel-cobalt-manganese) cathodes by a $H_2$ and C-reduction process. The recycled transition metal sulfate solutions are used in a co-precipitation process in a CSTR reactor to obtain the transition metal hydroxide. The NCM cathode materials (Ni:Mn:Co=5:3:2) are prepared from the transition metal hydroxide by calcining with lithium carbonate. X-ray diffraction and scanning electron microscopy analyses show that the cathode material has a layered structure and particle size of about 10 ${\mu}m$. The cathode materials also exhibited a capacity of about 160 mAh/g with a retention rate of 93~96% after 100 cycles.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.25 no.3
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• pp.116-120
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• 2015

$La_2NiO_{4+{\delta}}$ based oxides, a mixed electronic-ionic conductors (MIECs) with $K_2NiF_4$ type structure, have been considerably investigated in recent decades as electrode materials for advanced solid oxide fuel cells (SOFCs) due to their high electrical conductivity, and oxidation reduction reaction (ORR). In this study, structure properties of $La(Ca)_2Ni(Cu)O_{4+{\delta}}$ were studied as a potential cathode for intermediate temperature SOFCs (IT-SOFCs).

• Clean Technology
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• v.29 no.2
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• pp.87-94
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• 2023

The recovery of valuable metals from waste lithium-based secondary batteries is very important in terms of efficiently utilizing earth's limited number of resources. Currently, the cathode material of a LiFePO₄ battery, a type of battery which is widely used in automobiles, contains approximately 5% lithium. After use, the lithium in these batteries can be used again as a raw material for new batteries through lithium recycling. In this study, low-concentration sulfuric acid, a commonly used type of inorganic acid, was used to selectively leach the lithium contained in a waste LiFePO₄ cathode material powder. In addition, in order to compare and analyze the leaching efficiency and separation efficiency of each component, the optimalleaching conditions were derived by applying a two-step leaching process with pulp density being used as a variable during leaching. When leaching with pulp density as a variable, it was confirmed that at a pulp density of 200 g/L, the separation efficiency was approximately 200 times higher than at other pulp densities because the iron and phosphorus components were hardly leached at this pulp density. Accordingly, the pulp density of 200 g/L was used tooptimize the leaching conditions for the selective leaching and recovery of lithium.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.31 no.1
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• pp.16-23
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• 2021

Lithium carbonate recovered from the waste solution generated during the lithium secondary battery manufacturing process contains heavy metals such as cobalt, nickel, and manganese. In this study, the recrystallization of lithium carbonate was performed to remove heavy metals contained in the powder and to increase the purity of lithium carbonate. First, the leaching efficiency of lithium carbonate according to pH in the aqueous hydrochloric acid solution was examined, and the effect on the recrystallization of lithium carbonate according to the equivalent and concentration of sodium carbonate was confirmed. As the equivalent and concentration of sodium carbonate increased, the recovery rate of lithium carbonate improved. And the SEM image showed that the crystal shape was changed depending on the reaction conditions with sodium carbonate. Finally, the high purity lithium carbonate of 99.9% or more was recovered by washing with water.

• Journal of the Korean Ceramic Society
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• v.39 no.4
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• pp.359-366
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• 2002

The purpose of this study is to investigate the properties of LSGM electrolyte and LSM cathode. The unit cell based on the optimum conditions and processing for high performance was fabricated and measured. The single phase of $LaGaO_3$ was obtained on sintering at $1500^{\circ}$ for 6h with composition of $(La_{0.85}Sr_{0.15})(Ga_{0.8}Mg_{0.2})O_{3-\delta}와 (La_{0.8}Sr_{0.2})(Ga_{0.8}Mg_{0.2})O_{3-\delta}$ and $(La_{0.85}Sr_{0.15})(Ga_{0.8}Mg_{0.2})O_{3-\delta}$. The grain size of the sintered body was about $10∼30{\mu}m$ and electrical conductivity was 0.13 S/cm measured at $800^{\circ}$. The single phase of $LaMnO_3$ structure in $(La1-xSrx)MnO_3$ system was obtained at x=0∼0.2 and the particle size of the synthesized powder was about 40 nm. The unit cell was prepared by firing at $1200^{\circ}$ for 1h with $(La_{0.9}Sr_{0.1})MnO_3$ cathode and 0.9NiO-0.1YSZ anode screen-printed on surfaces of $(La_{0.8}Sr_{0.2})(Ga_{0.8}Mg_{0.2})O_{3-\delta}$ electrolyte. The grain size of the electrode was close to $1{\mu}m$ and the electrode had porous structure. The maximum power density of unit cell showed $0.3W/cm^2$ at $800^{\circ}$.