• Journal of Powder Materials
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• v.26 no.4
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• pp.340-344
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• 2019

Due to the rapid development of electricity, electronics, information communication, and biotechnology in recent years, studies are actively being conducted on nanopowders as it is required not only for high strengthening but also for high-function powder with electric, magnetic, and optical properties. Nonetheless, studies on nickel nanopowders are rare. In this study of the synthesis of nickel nanoparticles from $LiNiO_2$ (LNO), which is a cathode active material, we have synthesized the nanosized nickel powder by the liquid reduction process of $NiSO_4$ obtained through the leaching and purification of LNO. Moreover, we have studied the reduction reaction rate according to the temperature change of liquid phase reduction and the change of particle size as a function of NaOH addition amount using hydrazine monohydrate ($N_2H_4{\cdot}H_2O$) and NaOH.

• Resources Recycling
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• v.24 no.6
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• pp.9-16
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• 2015

In a recycling scheme of spent lithium ion batteries, a co-precipitation process for the re-synthesis of precursor is essential after the leaching of lithium ion battery scraps. In this study, the effect of ammonia as impurity during the co-precipitation process was investigated in order to re-synthesize a precursor of Ni-rich cathode active material $LiNi_{0.6}Co_{0.2}Mn_{0.2}O_2$ (NCM 622). As ammonia concentration increases from 1 M (the optimum condition for synthesis of the precursors based on 2 M of metal salt solution) to 4 M, the composition of obtained precursors deviates from the designed composition, most notably for Ni. The Ni co-precipitation efficiency gradually decreases from 100% to 87% when the concentration of ammonia solution increases from 1 M to 4 M. Meanwhile, the morphological properties of the obtained precursors such as sphericity, homogeneity and size distribution of particles were also investigated.

• Resources Recycling
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• v.28 no.4
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• pp.30-36
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• 2019

In this study, Li powder was recovered from the by-product of LNO ($Li_2NiO_2$) process, which is the positive electrode active material of waste lithium ion battery, through the $CO_2$ thermal reaction process. In the process of recovering Li powder, the $CO_2$ injection amount is 300 cc/min. The $Li_2NiO_2$ award was phase-separated into the $Li_2CO_3$ phase and the NiO phase by holding at $600^{\circ}C$ for 1 min. After this, the collected sample:distilled water = 1:50 weight ratio, and after leaching, the solution was subjected to vacuum filtration to recover $Li_2CO_3$ from the solution, and the NiO powder was recovered. In order to increase the purity of Ni, it was maintained in $H_2$ atmosphere for 3 hours to reduce NiO to Ni. Through the above-mentioned steps, the purity of Li was 2290 ppm and the recovery was 92.74% from the solution, and Ni was finally produced 90.1% purity, 92.6% recovery.

• Resources Recycling
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• v.16 no.6
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• pp.10-19
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• 2007

The mechanical process followed by hydrometallurgical treatment has been developed in order to recover cobalt and lithium from spent lithium ion battery. In the previous study, a citrate precursor combustion process to prepare cathodic active materials from the leaching solution was elucidated. Resynthesis of electrode materials should be more valuable in spent battery recycling. Conventional slurry mixing of $LiCoO_2$ and carbon cannot make uniform distribution, and therefore the cathode cannot reach the theoretical charge-discharge capacity and is easily degraded during the charge-discharge cycling. In this study, ultra-fine $LiCoO_2$ powders has been prepared by modification of the combustion process and fabricated the enhanced cathode by modification of mixing method of $LiCoO_2$ and carbon added.

• Resources Recycling
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• v.30 no.6
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• pp.36-42
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• 2021

Spent lithium-ion batteries are treated by reduction-smelting at high temperatures to recover valuable metals. Solvent extraction and precipitation of the HCl leaching solution of reduction-smelted metallic alloys resulted in a filtrate containing Ni(II) and a small amount of Si(IV). Adsorption and precipitation experiments were conducted to recover pure Ni(II) compounds from the filtrate. Si(IV) was selectively loaded onto polyacrylamide, but this method did not efficiently filter the solution due to an increase in viscosity. The addition of Na₂CO₃ as a precipitant to the filtrate led to the simultaneous precipitation of Ni(II) and Si(IV). However, it was possible to recover nickel oxalate with a purity higher than 99.99% by selectively precipitating Ni(II) with the addition of Na₂C₂O₄ as a precipitant.

• Resources Recycling
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• v.31 no.3
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• pp.73-80
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• 2022

Reduction smelting of spent lithium-ion batteries at high temperature produces metallic alloys. Following solvent extraction of the leaching solutions of these metallic alloys with either sulfuric or hydrochloric acid, the raffinate is found to contain Ni(II), Co(II), Mn(II), and Si(IV). In this study, two cationic exchange resins (Diphonix and P204) were employed to investigate the loading behavior of these ions from synthetic sulfate and chloride solutions. Experimental results showed that Ni(II), Co(II), and Mn(II) could be selectively loaded onto the Diphonix resin from a sulfate solution of pH 3.0. With a chloride solution of pH 6.0, Mn(II) was selectively loaded onto the P204 resin, leaving Ni(II) and Si(IV) in the effluent. Elution experiments with H₂SO₄ and/or HCl resulted in the complete recovery of metal ions from the loaded resin.

• Nuclear Engineering and Technology
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• v.54 no.6
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• pp.1962-1971
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• 2022

The liquid lead-lithium (Pb-17Li) blanket has many applications in fusion reactors due to its good tritium breeding performance, high heat transfer efficiency and safety. The compatibility of liquid Pb-17Li alloy with the structural material of blanket under magnetic field is one of the concerns. In this study, corrosion experiments China low activation martensitic (CLAM) steel and 316L steel were carried out in a forced convection Pb-17Li loop under 1.0 T magnetic field at 480 ℃ for 1000 h. The corrosion results on 316L steel showed the characteristic with a superficial porous layer resulted from selective leaching of high-soluble alloy elements and subsequent phase transformation from austenitic matrix to ferritic phase. Then the porous layers were eroded by high-velocity jet fluid. The main corrosion mechanism of CLAM steel was selective dissolution-base corrosion attack on the microstructure boundary regions and exclusively on high residual stress areas. CLAM steel performed a better corrosion resistance than that of 316L steel. The high Ni dissolution rate and the erosion of corroded layers are the main causes for the severe corrosion of 316L steel.

• Environmental Engineering Research
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• v.25 no.1
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• pp.88-95
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• 2020

An investigation of rare metals recovery from LiNi_xCo_yMn_zO₂ cathode material of the end-of-life lithium-ion batteries is presented. To determine the influence of reductant on the leach process, the cathode material (containing Li 7.6%, Co 20.4%, Mn 19.4%, and Ni 19.3%) was leached in H₂SO₄ solutions either with or without H₂O₂. The optimal process parameters with respect to acid concentration, addition dosage of H₂O₂, temperature, and the leaching time were found to be 2.0 M H₂SO₄, 4 vol.% H₂O₂, 70℃, and 150 min, respectively. The yield of metal values in the leach liquor was > 99%. The leach liquor was subsequently treated by precipitation techniques to recover nickel as Ni(C₄H₇N₂O₂)₂ and lithium as Li₂CO₃ with stoichiometric ratios of 2:1 and 1.2:1 of dimethylglyoxime:Ni and Na₂CO₃:Li, respectively. Cobalt was recovered by solvent extraction following a 3-stage process using Na-Cyanex 272 at pH_eq ~5.0 with an organic-to-aqueous phase ratio (O/A) of 2/3. The loaded organic phase was stripped with 2.0 M H₂SO₄ at an O/A ratio of 8/1 to yield a solution of 114 g/L CoSO₄; finally recovered CoSO₄.xH₂O by crystallization. The process economics were analyzed and found to be viable with a margin of $476 per ton of the cathode material.

• Resources Recycling
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• v.31 no.5
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• pp.34-41
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• 2022

Smelting reduction of spent lithium-ion batteries results in metallic alloys, slag, and dust containing Li(I). Precipitation of Li₂CO₃ was performed using the synthetic leachate of the dust. Herein, the effects of the precipitant and addition of non-aqueous solvents on the precipitation of Li(I) were investigated. Na₂CO₃ was a more effective precipitating agent than (NH₄)₂CO₃ owing to the hydrolysis reaction of dissolved ammonium and carbonate. The addition of acetone or ethanol improved the Li(I) precipitation percentage for both the precipitants. When using (NH₄)₂CO₃, the Li(I) precipitation percentage increased at a solution pH of 12. Under the same conditions, the Li(I) precipitation percentage using Na₂CO₃ was much higher than that using (NH₄)₂CO₃.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.12 no.10
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• pp.4660-4665
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• 2011

New precursors as a Li adsorbent, $Li_{1.6}(MnM)_{1.6}O_4$ (M=Cu, Ni, Co, Fe), were synthesized by hydrothermal method and their physicochemical properties were discussed. XRD and HRTEM results revealed that the original spinel structure was stabilized by cobalt-doping while Cu-, Ni- and Fe-doping led to structural changes. Such a structural stabilization by Cobalt-doping was maintained after lithium leaching by acid treatment. Li absorption efficiency from seawater was significantly enhanced by using the Cobalt-doped spinel manganese oxide, $Li_{1.6}[MnCo]_{1.6}O_4$, compared to the commercially available $Li_{1.33}Mn_{1.67}O_4$; the adsorbed amount of Li from 1g-adsorbent was 35 and 16 mg by $Li_{1.6}[MnCo]_{1.6}O_4$, and $Li_{1.33}Mn_{1.67}O_4$, respectively.