• Resources Recycling
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• v.32 no.3
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• pp.9-17
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• 2023

Efforts are currently underway to develop a method for efficiently recovering lithium from the cathode material of waste lithium iron phosphate batteries (LFP). The successful application of lithium battery recycling can address the regional ubiquity and price volatility of lithium resources, while also mitigating the environmental impact associated with both waste battery material and lithium production processes. The isomorphic substitution leaching process was used to recover lithium from spent lithium iron phosphate batteries. Lithium was leached by the isomorphic substitution of Fe²⁺ in LFP using a relatively inexpensive ferric chloride etching solution as a leaching agent. In the study, the leaching rate of lithium was compared using the ferric chloride etching solution at various multiples of the LFP molar ratio: 0.7, 1.0, 1.3, and 1.6 times. The highest lithium leaching rate was shown at about 98% when using 1.3 times the LFP molar ratio. Subsequently, to eliminate Fe, the leachate was treated with NaOH. The Fe-free solution was then used to synthesize lithium carbonate, and the harvested powder was characterized and validated. The surface shape and crystal phase were analyzed using SEM and XRD analysis, and impurities and purity were confirmed using ICP analysis.

• Journal of the Korean institute of surface engineering
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• v.55 no.4
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• pp.231-235
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• 2022

As environmental pollution becomes more serious, the demand for electric vehicles (EVs) and lithium-ion batteries for electric vehicles is rapidly increasing worldwide. Accordingly, the amount of waste batteries is also increasing, and a technology for recycling and reusing them is required. In order to reuse a used battery, it is necessary to non-destructively diagnose the deterioration condition of the battery. Therefore, in this study, we investigate the diagnosis of degradation for parallel-connected lithium-ion battery cells through non-constructive electrochemical approach. As the number of parallel-connected cells increased, in addition to linear degradation, abrupt step-like degradation occurred, which is attributed to the predominant degradation of specific cells. In addition, it is confirmed that deteriorated cells among multiple cells can be distinguished through a simple measurement of open circuit voltage (OCV).

• Resources Recycling
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• v.32 no.1
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• pp.21-32
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• 2023

Because the application of lithium has gradually increased for the production of lithium ion batteries (LIBs), more research studies about recycling using solvent extraction (SX) should focus on Li⁺ recovery from the waste solution obtained after the removal of the valuable metals nickel, cobalt and manganese (NCM). The raffinate obtained after the removal of NCM metal contains lithium ions and other impurities such as Na ions. In this study, we optimized a selective SX system using di-(2-ethylhexyl) phosphoric acid (D2EHPA) as the extractant and tri-n-butyl phosphate (TBP) as a modifier in kerosene for the recovery of lithium from a waste solution containing lithium and a high concentration of sodium (Li⁺ = 0.5 ~ 1 wt%, Na⁺ = 3 ~6.5 wt%). The extraction of lithium was tested in different solvent compositions and the most effective extraction occurred in the solution composed of 20% D2EHPA + 20% TBP + and 60% kerosene. In this SX system with added NaOH for saponification, more than 95% lithium was selectively extracted in four extraction steps using an organic to aqueous ratio of 5:1 and an equilibrium pH of 4 ~ 4.5. Additionally, most of the Na⁺ (92% by weight) remained in the raffinate. The extracted lithium is stripped using 8 wt% HCl to yield pure lithium chloride with negligible Na content. The lithium chloride is subsequently treated with high purity ammonium bicarbonate to afford lithium carbonate powder. Finally the lithium carbonate is washed with an adequate amount of water to remove trace amounts of sodium resulting in highly pure lithium carbonate powder (purity > 99.2%).

• 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.

• 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.

• Resources Recycling
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• v.30 no.1
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• pp.44-52
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• 2021

This study investigated the effect of the type of alkaline precipitant used on the synthesis of lithium hydroxide by examining the behavior of lithium hydroxide produced using lithium sulfate recovered from a waste lithium secondary battery as a raw material. The double-replacement reaction (DRR) process was used to remove the impurities contained in the lithium salt precursor of lithium sulfate and to improve the efficiency of the synthesis of lithium hydroxide. The experiment was conducted by control the molar ratio of the precursor ([Li]/[OH]), the reaction temperature, and the composition of the alkaline precipitant (KOH, Ca(OH)2, Ba(OH)2) used for the production of highly-crystalline lithium hydroxide. A secondary solid-liquid separation was performed following the reaction to remove the impurities generated, and the purified aqueous solution of lithium hydroxide was evaporated to remove the moisture and obtain the product as a powder. The crystallinity and synthesis behavior of the product were examined.

• Applied Chemistry for Engineering
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• v.30 no.3
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• pp.290-296
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• 2019

Lithium-ion batteries are one of the most interesting devices in a number of energy storage systems. In particular, the usage of energy storage devices is increasing due to an increase in demand for renewable energy as a distributed power supply source, stable supply of electric power, and expansion of electric vehicles. Of late, the recycling and restoration technology of waste lithium ion batteries due to the increase in its usage amount as the energy storage system is a socially and economically important research field. In this review, we intend to describe the performance diagnosis, recycling or restoration technology of lithium ion battery and its potential development.

• Journal of the Korean Recycled Construction Resources Institute
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• v.10 no.4
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• pp.547-552
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• 2022

In this study, we secured a technology for manufacturing expanded glass of uniform quality by using general tempered glass, that is, window glass, among automotive glass that is scrapped, and verified whether the manufactured expanded glass can be used for lithium battery fire suppression. The process of manufacturing expanded glass using waste glass is generally divided into Crushing → Milling → Granulation → Expansion → Cooling. With several trials a nd errors. It is obtained a yield of 0.5 ø mm to 2 ø mm spherical particles of 80 % or more. By comparing the surface analysis and physical properties, a more suitable sample was selected as a fire extinguishing agent for lithium batteries, and it was confirmed that the result of the adaptability test for lithium battery fire was satisfactory.

• Journal of the Microelectronics and Packaging Society
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• v.27 no.4
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• pp.83-89
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• 2020

For the past few decades, as part of efforts to protect the environment where fossil fuels, which have been a key energy resource for mankind, are becoming increasingly depleted and pollution due to industrial development, ecofriendly secondary batteries, hydrogen generating energy devices, energy storage systems, and many other new energy technologies are being developed. Among them, the lithium-ion battery (LIB) is considered to be a next-generation energy device suitable for application as a large-capacity battery and capable of industrial application due to its high energy density and long lifespan. However, considering the growing battery market such as eco-friendly electric vehicles and drones, it is expected that a large amount of battery waste will spill out from some point due to the end of life. In order to prepare for this situation, development of a process for recovering lithium and various valuable metals from waste batteries is required, and at the same time, a plan to recycle them is socially required. In this study, we introduce a nanoscale pattern transfer printing (NTP) process of Li2CO3, a representative anode material for lithium ion batteries, one of the strategic materials for recycling waste batteries. First, Li2CO3 powder was formed by pressing in a vacuum, and a 3-inch sputter target for very pure Li2CO3 thin film deposition was successfully produced through high-temperature sintering. The target was mounted on a sputtering device, and a well-ordered Li2CO3 line pattern with a width of 250 nm was successfully obtained on the Si substrate using the NTP process. In addition, based on the nTP method, the periodic Li2CO3 line patterns were formed on the surfaces of metal, glass, flexible polymer substrates, and even curved goggles. These results are expected to be applied to the thin films of various functional materials used in battery devices in the future, and is also expected to be particularly helpful in improving the performance of lithium-ion battery devices on various substrates.

• Resources Recycling
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• v.14 no.6 s.68
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• pp.37-43
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• 2005

[ $LiCoO_{2}$ ] nanoparticles were synthesized from leach liquor of lithium ion battery waste using flame spray pyrolysis. Electrode Materials containing lithium and cobalt could be concentrated with thermal and mechanical treatment. After dissolution of used cathode materials of the lithium battery with nitric acid, the molar ratio of Li/Co in the leach liquor was adjusted at 1.0 by adding a fresh $LiNO_{3}$ solution. The nanoparticles synthesized by the flame spray pyrolysis showed clear crystallinity and were nearly spherical, and their average primary particle diameters ranged from 11 to 35 nm. The average particle diameter increased with an increase in the molar concentration of the precursor. Raising the maximum flame temperature by controlling the gas flow rates also led to an increase in the average diameter of the particles. The $LiCoO_{2}$ powder was proved to have good characteristics as cathode active materials in charge/discharge capacity and cyclic performance.