• Bulletin of the Korean Chemical Society
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• v.34 no.3
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• pp.851-855
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• 2013

This paper describes an environmentally friendly process for the recovery of $LiFePO_4$ cathode materials from scrap electrodes by a simple thermal treatment method. The active materials were easily separated from the aluminum substrate foil and polymeric binders were also decomposed at different temperatures ($400^{\circ}C$, $500^{\circ}C$, $600^{\circ}C$) for 30 min under nitrogen gas flow. The samples were characterized by X-ray diffraction (XRD), scanning electronic microscopy (SEM), Raman spectroscopy, Thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). The electrochemical properties of the recycled $LiFePO_4$ cathode were evaluated by galvanostatic charge and discharge modes. The specific charge/discharge capacities of the recycled $LiFePO_4$ cathode were similar to those of the original $LiFePO_4$ cathode. The $LiFePO_4$ cathode material recovered at $500^{\circ}C$ exhibits a somewhat higher capacity than those of other recovered materials at high current rates. The recycled $LiFePO_4$ cathode also showed a good cycling performance.

• Korean Chemical Engineering Research
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• v.53 no.2
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• pp.137-144
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• 2015

The present paper deals with the extractive separation and selective recovery of nickel and lithium from the sulfate leachate of cathode scrap generated during the manufacture of LIBs. The conditions for extraction, scrubbing and stripping of nickel from lithium were optimized with an aqueous feed containing $2.54kg{\cdot}m^{-3}$ Ni and $4.82kg{\cdot}m^{-3}$ Li using PC-88A. Over 99.6% nickel was extracted with $0.15kmol{\cdot}m^{-3}$ PC-88A in two counter-current stages at O/A=1 and pH=6.5. Effective scrubbing Li from loaded organic was systematically studied with a dilute $Na_2CO_3$ solution ($0.10kmol{\cdot}m^{-3}$). The McCabe-Thiele diagram suggests two counter-current scrubbing stages are required at O/A=2/3 to yield lithium-scrubbing efficiency of 99.6%. The proposed process showed advantages of simplicity, and high purity (99.9%) nickel sulfate recovery along with lithium to ensure the complete recycling of the waste from LIBs manufacturing process.

• 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 Powder Materials
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• v.28 no.6
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• pp.497-501
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• 2021

Cobalt (Co) is mainly used to prepare cathode materials for lithium-ion batteries (LIBs) and binder metals for WC-Co hard metals. Developing an effective method for recovering Co from WC-Co waste sludge is of immense significance. In this study, Co is extracted from waste cemented carbide soft scrap via mechanochemical milling. The leaching ratio of Co reaches approximately 93%, and the leached solution, from which impurities except nickel are removed by pH titration, exhibits a purity of approximately 97%. The titrated aqueous Co salts are precipitated using oxalic acid and hydroxide precipitation, and the effects of the precipitating agent (oxalic acid and hydroxide) on the cobalt microstructure are investigated. It is confirmed that the type of Co compound and the crystal growth direction change according to the precipitation method, both of which affect the microstructure of the cobalt powders. This novel mechanochemical process is of significant importance for the recovery of Co from waste WC-Co hard metal. The recycled Co can be applied as a cemented carbide binder or a cathode material for lithium secondary batteries.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.13 no.1
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• pp.11-19
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• 2015

The production of nuclear fuel cladding tube is expected to increase with the nuclear power plant expansion. Zirconium(Zr) scrap that is generated during manufacturing is also expected to increase. Zr electrorefining experiment was carried out in the fluoride salt of LiF-KF-ZrF₄ using multiple electrode for scale up and improving throughput Zr electrorefiner develop-ment. The Zr reduction peak observed at-0.8 V(vs.Ni). Polarization behavior showed that the amount of applied current increases because of decreasing cell resistance as the number of cathode increases. Experimental results showed the highest recovery rate about 98% at lowest current density of 25.64 mA/cm² using 6 electrodes. XRD and TG analysis result show that pure Zr was recovered 99.92% and ICP analysis shows that lower impurity content than conventional impurity content of the Anode(97.8%). Electrorefining consumes energy about 7.15 kWh/kg less than 39.7% compared to the Kroll process using 6 electrode width of 20 mm and height of 65 mm. Because of increasing cell efficiency and recovery rate, using multiple cathode is determined as an efficient technique for scale up electrorefining Zr scrap.

• Journal of the Korean Electrochemical Society
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• v.17 no.2
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• pp.111-118
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• 2014

The electrochemical properties using the cells assembled with the synthesized $LiCoO_2$(LCO) were evaluated in this study. The LCO was synthesized from high-purity cobalt sulfate($CoSO_4$) which is recovered from the cathode scrap in the wastes lithium ion secondary battery(LIB). The leaching process for dissolving the metallic elements from the LCO scrap was controlled by the quantities of the sulfuric acid and hydrogen peroxide. The metal precipitation to remove the impurities was controlled by the pH value using the caustic soda. And also, D2EHPA and $CYANEX^{(R)}272$ were used in the solvent extraction process in order to remove the impurities again. The high-purity $CoSO_4$ solution was recovered by the processes mentioned above. We made the 6 wt.% $CoSO_4$ solution mixed with distilled water. And the 6 wt.% $CoSO_4$ solution was mixed with oxalic acid by the stirring method and dried in oven. $LiCoO_2$ as a cathode material for LIB was formed by the calcination after the drying and synthesis with the $Li_2CO_3$ powder. We assembled the cells using the $LiCoO_2$ powders and evaluated the electrochemical properties. And then, we confirmed possibility of the recyclability about the cathode materials for LIBs.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.13 no.4
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• pp.315-319
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• 2015

A high-throughput electrorefiner has been developed for commercialization use by enhancing the uranium recovery from the reduced metal which is produced from the oxide reduction process. It is necessary to scrap and effectively collect uranium dendrites from the surface of the solid cathode for high yield. When a steel electrode is used as the cathode in the electrorefining process, uranium is deposited and regularly stuck to the steel cathode during electrorefining. The sticking coefficient of a steel cathode is very high. In order to decrease the sticking coefficient of the steel cathode effectively, vibration mode was applied to the electrode in this study. Uranium dendrites were scraped and fell apart from the steel cathode by a vibration force. The vibrational scraping of the steel cathode was compared to the self-scraping of the graphite cathode. Effects of the applied current density and the vibration stroke on the scraping of the uranium dendrites were also investigated.

• Applied Chemistry
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• v.16 no.1
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• pp.73-76
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• 2012

Due to the developments of communications equipment and electronic devices, lithium ion secondary battery usage is growing. Along with demand increasing, the amount of scrap has been steadily increasing. In this study, method of cobalt recovery using organic eco-friendly is proposed. Sulfuric acid, Malic acid, Citric acid at reflux device had good cobalt leaching efficiency. And Sulfuric acid, Malic acid at the autoclave increased cobalt leaching efficiency.

• Resources Recycling
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• v.28 no.1
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• pp.3-14
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• 2019

Copper is used in many electronic components and construction parts due to its excellent electrical conductivity and heat transfer characteristics, and also used for pre-plating for double layer coating such as nickel, so that copper is an essential material in modern industry. Despite the expected increase of usage and importance on wiring, sensors and data equipment in the next generation industries, it is hard for securing stable copper supply and resource management resulting from the copper prices are fluctuating owing to the economic crisis in Europe, the low economic growth trend in China, and President Trump's commitment to public industrial facilities investment in U.S.. Since most of the domestic copper consumption is used by electrolytic copper cathode, we studied not only copper recycling technology which is being commercialized but also current research trend under the research stage. This study aims to examine the characteristics of each process and the areas where future recycling technology development is required.

• Resources Recycling
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• v.32 no.6
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• pp.25-33
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• 2023

With the growth of the battery industry, a rapid increase in the production and usage of lithium-ion batteries is expected, and in line with this, much interest and effort is being paid to recycle waste batteries, including production scrap. Although much effort has been made to recycle cathode material, much attention has begun to recycle anode material to secure the supply chain of critical minerals and improve recycling rates. The proximate analysis that measures the content of coal can be used to analyze graphite in anode material, but it cannot accurately analyze due to the interaction between the components of the black mass. Therefore, in this study, thermogravimetric analysis of each component of black mass was measured as the temperature increased up to 950℃ in an oxygen atmosphere. As a result, in the case of cathode material, no change in mass was measured other than a mass reduction of about 5% due to oxidation of the binder and conductive material. In the case of anode material, except for a mass reduction of about 2% due to the binder, all mass reduction were due to the graphite(fixed carbon). In addition, metal conductors (Al, Cu) were oxidized and their mass increased as the temperature increased. Thermal analysis results of mixed samples of cathode/anode show similar results to the predictive values that can be calculated through each cathode and anode analysis results.