• Clean Technology
• /
• v.20 no.3
• /
• pp.277-282
• /
• 2014

In this study, PU-LMO was made by immobilization of LMO on urethane foam (PU) with using an EVA as a binder. PU-LMO was characterized by using X-Ray Diffractometer (XRD) and Scanning Electron Microscopy (SEM). The optimal ratio of EVA/LMO for preparation of PU-LMO was 0.26 gEVA/gLMO. The adsorption of lithium ions by PU-LMO was found to follow the pseudo-second-order kinetic model. The equilibrium data fitted well with Langmuir isotherm model and the maximum removal capacity of lithium ions was 17.09 mg/g. The PU-LMO was found to have a remarkably high selectivity of lithium ions and high adsorption capacity because the distribution coefficient ($K_d$) of lithium ion was higher than those of other metal ions.

• Bulletin of the Korean Chemical Society
• /
• v.31 no.2
• /
• pp.309-314
• /
• 2010

The surface modified $LiMn_2O_4$ materials with Li-Fe composites were prepared by a sol-gel method to improve the electrochemical performance of $LiMn_2O_4$ and were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS), and transmission electron microscopy (TEM)-EDS. XRD results indicate that all the samples (modified and pristine samples) have cubic spinel structures, and XRD, XPS, and TEM-EDS data reveal the formation of $Li(Li_xFe_xMn_{2-2x})O_4$ solid solution on the surface of particles. For the electrochemical properties, the modified material demonstrated dramatically enhanced reversibility and stability even at elevated temperature. These improvements are attributed to the formation of the solid solution, and thus-formed solid solution phase on the surface of $LiMn_2O_4$ particle reduces the dissolution of Mn ion and suppresses the Jahn-Teller effect.

• Journal of the Korean Ceramic Society
• /
• v.48 no.5
• /
• pp.379-383
• /
• 2011

This paper presents the synthesis of one-dimensional spinel $LiMn_2O_4$ nanostructures using a facile and scalable two-step process. $LiMn_2O_4$ nanorods with average diameter of 100 nm and length of 1.5 ${\mu}m$ have been prepared by solid-state lithiation of hydrothermally synthesized ${\beta}$-$MnO_2$ nanorods. $LiMn_2O_4$ nanowires with diameter of 10 nm and length of several micrometers have been fabricated via solid-state lithiation of ${\beta}$-$MnO_2$ nanowires. The precursors have been lithiated with LiOH and reaction temperature and pressure have been controlled. The complete structural transformation to cubic phase and the maintenance of 1-D nanostructure morphology have been evaluated by XRD, SEM, and TEM analysis. The size distribution of the spinel $LiMn_2O_4$ nanorods/wires has been similar to the $MnO_2$ precursors. By control of reaction pressure, cubic 1-D spinel $LiMn_2O_4$ nanostructures have been fabricated from tetragonal $MnO_2$ precursors even below $500^{\circ}C$.

• Resources Recycling
• /
• v.22 no.4
• /
• pp.62-69
• /
• 2013

A study on the recovery of lithium and leaching behavior of NCM powder by carbon reduction for NCM-system Li-ion battery scraps was conducted. First of all, the oxide powders of NCM-system with layer structure were decomposed by carbon, lithium was converted to lithium carbonate by carbon reaction at above $600^{\circ}C$. The lithium carbonate powders with 99% purity were manufactured by washing method with water and concentration process for NCM powder after carbon reduction. The reaction yield was approximately 88% at $800^{\circ}C$ by carbon reduction. At this time, leaching efficiency at 2M sulfuric acid concentration was over 99% for cobalt, nickel and manganese.

• Resources Recycling
• /
• v.16 no.3 s.77
• /
• pp.50-60
• /
• 2007

There are several kinds of battery such as zinc-air battery, lithium battery, Manganese dry battery, silver oxide battery, mercury battery, sodium-sulphur battery, lead battery, nickel-hydrogen secondary battery, nickel-cadmium battery, lithium ion battery, alkaline battery, etc. These days it has been widely studied for the recycling technologies of the used battery from view points of economy and efficiency. In this paper, patents on the recycling technologies of the used lithium battery were analyzed. The range of search was limited in the open patents of USA(US), European Union(EP), Japan(JP), and Korea(KR) from 1986 to 2006. Patents were collected using key-words searching and filtered by filtering criteria. The trends of the patents was analyzed by the years, countries, companies, and technologies.

• Korean Chemical Engineering Research
• /
• v.51 no.4
• /
• pp.460-464
• /
• 2013

A series of Mn compound were prepared by seed-assisted method. The seed used in this reaction was manufactured by calcination of $MnCO_3$ at various temperatures and effects of the calcination temperature on seed-assisted reaction were investigated. With increase of the calcination temperature, CMD (${\gamma}-MnO_2$) was recovered after seed-assisted reactions. LMO used as cathode active material in the Li-ion batteries were synthesized from Mn source obtained in the seed-assisted reaction and the electrochemical properties (rate capability, cycle life performance and specific capacity) of the LMO were investigated. The LMO synthesized from the CMD which is obtained by the reaction with seed prepared by calcination of $MnCO_3$ more than $350^{\circ}C$ shown good electrochemical properties.

• Journal of the Korean Electrochemical Society
• /
• v.15 no.2
• /
• pp.67-73
• /
• 2012

Spherical lithium manganese oxide spinel, $LiMn_{2-x}M_xO_4$ (M = Al, Mg, B) prepared by wet-milling, spray-drying, and sintering process has been investigated as a cathode material for lithium ion batteries. As-prepared powders exhibit various surface morphologies and internal density in terms of boron (B) doping level. It is found that the dopant B drives the growth of the primary particle and minimizes the surface area of the powder. As a result, the dopant enhances the internal density of the particles. Electrochemical tests demonstrated that the capacity of the synthesized material at 5 C could be maintained up to 90% of that at 0.2 C. The cycle performance of the material showed that the initial capacity was retained up to 80% even after 500 cycles under the high temperature of $60^{\circ}C$.

• Bulletin of the Korean Chemical Society
• /
• v.34 no.2
• /
• pp.622-628
• /
• 2013

Nanocrystalline spinel lithium manganese oxide ($LiMn_2O_4$) powders with narrow-size-distribution, pure-phase particles, and high crystallinity with an average crystallite size of about 70 nm were synthesized at $600^{\circ}C$ for 6 h in air by freeze drying method. Spinel $LiMn_2O_4$ is also prepared by sol-gel using citric acid as a chelating agent. The influence of different parameters such as pH conditions, solvent, molar ratio of citric acid to total metal ions, calcination temperature, starting material on the structure, morphology and purity of this oxide was investigated. The results of sol-gel method show that pure $LiMn_2O_4$ with average crystallite size of about 130 nm can be produced from nitrate salts as starting materials at $800^{\circ}C$ for 6 h in air. The optimum pH and molar ratio of chelating agent to total metal ions are $4{\leq}pH{\leq}6$ and 1.0, respectively. A possible mechanism on the formation of the nanocrystallines synthesized by sol-gel was also discussed. At the end a comparison of the differences between two methods was made on the basis of x-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA) tests.

• Resources Recycling
• /
• v.30 no.6
• /
• pp.43-52
• /
• 2021

In this study, the optimal nitration process for selective lithium leaching from powder of a spent battery cell (LiNi_xCo_yMn_zO₂, LiCoO₂) was studied using Taguchi method. The nitration process is a method of selective lithium leaching that involves converting non-lithium nitric compounds into oxides via nitric acid leaching and roasting. The influence of pretreatment temperature, nitric acid concentration, amount of nitric acid, and roasting temperature were evaluated. The signal-to-noise ratio and analysis of variance of the results were determined using L₁₆(4⁴) orthogonal arrays. The findings indicated that the roasting temperature followed by the nitric acid concentration, pretreatment temperature, and amount of nitric acid used had the greatest impact on the lithium leaching ratio. Following detailed experiments, the optimal conditions were found to be 10 h of pretreatment at 700℃ with 2 ml/g of 10 M nitric acid leaching followed by 10 h of roasting at 275℃. Under these conditions, the overall recovery of lithium exceeded 80%. X-ray diffraction (XRD) analysis of the leaching residue in deionized water after roasting of lithium nitrate and other nitrate compounds was performed. This was done to determine the cause of rapid decrease in lithium leaching rate above a roasting temperature of 400℃. The results confirmed that lithium manganese oxide was formed from lithium nitrate and manganese nitrate at these temperatures, and that it did not leach in deionized water. XRD analysis was also used to confirm the recovery of pure LiNO₃ from the solution that was leached during the nitration process. This was carried out by evaporating and concentrating the leached solution through solid-liquid separation.

• Journal of the Korean Electrochemical Society
• /
• v.19 no.2
• /
• pp.50-56
• /
• 2016

Spherical lithium manganese oxide spinel, $Li_{1.10}Mn_{1.86}Al_{0.02}Mg_{0.02}O_4$ was prepared by wet-milling, spray-drying, and sintering process. In the spray-drying process, solid content in slurry was varied from 20 to 30 wt%. In the sintering process, the precursors have been sintered under air or $O_2$ atmosphere. While the as-prepared samples exhibit excellent electrochemical properties at room temperature, the discharge voltage profiles at 5.0C are very different one from another. The origin for the difference especially at initial state of discharge is oxygen defect. The sample prepared in air has larger capacity related to the plateau at 3.3 V (vs. $Li/Li^+$) which is caused by the oxygen defects than the one prepared in $O_2$. The difference of discharge voltage profiles especially at the final state of discharge comes from different diffusion rate of $Li^+$ ions. The sample prepared from 30 wt% solid content of slurry shows twice higher diffusion rate than the samples prepared from 20 wt% solid content, which is attributed to better compactness between primary particles for the sample prepared from 30wt % solid content than the one prepared by 20 wt%.