• Korean Chemical Engineering Research
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• v.56 no.6
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• pp.901-908
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• 2018

Graphite is used as a sample anode active material. However, since the maximum theoretical capacity is limited to $372mA\;h\;g^{-1}$, a new anode active material is required for the development of a high capacity lithium ion battery. The maximum theoretical capacity of Si is $4200mA\;h\;g^{-1}$, which is higher than that of graphite. However, it is not suitable for direct application to the anode active material because it has a volume expansion of 400%. In order to minimize the decrease of the discharge capacity due to the volume expansion, the Si was pulverized by the dry method to reduce the mechanical stress and the volume change of the reaction phase, and the change of the volume was suppressed by coating the carbon layers to the particle size controlled Si particles. And carbon fiber is grown like a thread on the particle surface to control secondary volume expansion and improve electrical conductivity. The physical and chemical properties of the materials were measured by XRD, SEM and TEM, and their electrochemical properties were evaluated. In this study, we have investigated the synthesis method that can be used as anode active material by improving cycle characteristics of Si.

• Korean Chemical Engineering Research
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• v.61 no.3
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• pp.348-355
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• 2023

Magnesium secondary batteries are attracting much attention due to their potential to replace conventionally used lithium ion batteries. Magnesium secondary battery cathode material Mo₆S₈ were synthesized by molten salt synthesis method and PVC as a carbon materials were added to improve electrochemical properties. Crystal structure, size and surface of the synthesized anode materials were measured through XRD and SEM. Charge-discharge profiles and rate capabilities were measured by battery test system. 2.81 wt% PVC coated sample showed the best rate capabilities of 85.8 mAh/g at 0.125 C-rate, 69.2 mAh/g at 0.5 C-rate, and 60.5 mAh/g at 1 C-rate.

• Journal of Powder Materials
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• v.23 no.2
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• pp.136-142
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• 2016

As precursors of cathode materials for lithium ion batteries, $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$ powders are prepared in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH in the presence of $NH_4OH$ in air or nitrogen ambient. Calcination of the precursors with $Li_2CO_3$ for 8 h at $1,000^{\circ}C$ in air produces dense spherical cathode materials. The precursors and final powders are characterized by X-ray diffraction (XRD), scanning electron microscopy, particle size analysis, tap density measurement, and thermal gravimetric analysis. The precursor powders obtained in air or nitrogen ambient show XRD patterns identified as $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$. Regardless of the atmosphere, the final powders exhibit the XRD patterns of $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ (NCM). The precursor powders obtained in air have larger particle size and lower tap density than those obtained in nitrogen ambient. NCM powders show similar tendencies in terms of particle size and tap density. Electrochemical characterization is performed after fabricating a coin cell using NCM as the cathode and Li metal as the anode. The NCM powders from the precursors obtained in air and those from the precursors obtained in nitrogen have similar initial charge/discharge capacities and cycle life. In conclusion, the powders co-precipitated in air can be utilized as precursor materials, replacing those synthesized in the presence of nitrogen injection, which is the usual industrial practice.

• Clean Technology
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• v.20 no.4
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• pp.433-438
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• 2014

There is an increasing interest in the development of rechargeable batteries suitable for use in both hybrid electric vehicles and energy storage systems that require higher charge & discharge rates, bigger battery sizes and increased safety of the batteries. Spinel-type lithium titanium oxide ($Li_4Ti_5O_{12}$) as a potential anode for lithium ion batteries has many advantages. It is a zero-strain materials and it experiences no structural change during the charge/discharge precess. Thus, it has long cycle life due to its structural integrity. It also offers a stable operation voltage of approximately 1.55 V versus $Li^+/Li$, above the reduction potential of most organic electrolyte. In this study, Ru added $Li_4Ti_5O_{12}$ composites were synthesized by solid state process. The characteristics of active material were investigated with TGA-DTA, XRD, SEM and charge/discharge test. The capacity was reduced when Ru was added, however, the polarization decreased. The capacity rate of $Li_4Ti_5O_{12}$ with Ru (3%, 4%) addition was reduced during the charge/discharge precess with 10 C-rate as a high current density.

• 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 the Korean Electrochemical Society
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• v.14 no.1
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• pp.27-32
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• 2011

The electorchemical properties of $Li_4Ti_5O_{12}$ added with Cr was tested. The addition or substitution of atoms to $Li_4Ti_5O_{12}$ are expected to modify the crystal structure, and therefore to change the electrochemical performances of $Li_4Ti_5O_{12}$. After the spinel structure $Li_4Ti_{5-x}Cr_xO_{12}$ (x = 0~0.2) were obtained via sol-gel method, the gel was heated in a muffle furnace at $800{\sim}850^{\circ}C$ for 12 h in air. The physical properties of the samples were characterized by TG-DTA, XRD, SEM, FT-IR, and the electrochemical properties were tested with battery cycler at 0.01~2.0 V range. The $Li_4Ti_5O_{12}$ exhibited 169.9 mAh/g at 1C and capacity recovery was 97.5% of the initial capacity at 0.1C. $Li_4Ti_{4.9}Cr_{0.1}O_{12}$ (Cr 1% added) showed best performance of 193.8 mAh/g at 1C and the capacity recovery was increased to 98.8% of the initial capacity at 0.1C.

• 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.

• Korean Chemical Engineering Research
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• v.60 no.3
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• pp.446-451
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• 2022

In this study, to improve capacity and cycle stability, the pitch coated nano silicon sheets/CNT composites were prepared through electrostatic bonding of nano silicon sheets and CNT. Silica sheets were synthesized by hydrolyzing TEOS on the crystal planes of NaCl, and then nano silicon sheets were prepared by using magnesiothermic reduction method. To fabricate the nano silicon sheets/CNT composites, the negatively charged CNT after the acid treatment was used to assemble the positively charged nano silicon sheets modified with APTES. THF as a solvent was used in the coating process of PFO pitch. The physical properties of the prepared anode composites were analysed by FE-SEM, XRD and EDS. The electrochemical performances of the synthesized anode composites were performed by current charge/discharge, rate performances, differential capacity and EIS tests in the electrolyte LiPF₆ dissolve solvent (EC:DMC:EMC = 1:1:1 vol%). It was found that the anode material with high capacity and stability could be synthesized when high composition of silicon and conductivity of CNT were used. The pitch coated nano silicon sheets/CNT anode composites showed initial discharge capacity of 2344.9 mAh/g and the capacity retention ratio of 81% after 50 cycles. The electrochemical property of pitch coated anode material was more improved than that of the nano silicon sheets/CNT composites.

• Journal of the Korean Electrochemical Society
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• v.15 no.2
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• pp.101-108
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• 2012

The purpose of this study was to improve the conductivity of $Li_3V_2(PO_4){_3}$ by adding carbon source so that the discharge rate and cyclic properties were improved. Glucose and CNT were added to $Li_3V_2(PO_4){_3}$ and the structure and electrochemical properties were studied. $Li_3V_2(PO_4){_3}$, $Li_3V_2(PO_4){_3}$/C and $Li_3V_2(PO_4){_3}$/CNT were synthesised by solid state reaction using hydrogen reduction method at 600, 700, 800, $900^{\circ}C$. The cathode materials were assembled to coin cell type 2032 with Lithium metal as a counter electrode. The coin cell was galvanostatically evaluated in the voltage range of 3.0~4.8 V.

• Journal of Powder Materials
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• v.23 no.4
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• pp.287-296
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• 2016

$Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$ powders have been synthesized in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH using $NH_4OH$ as a chelating agent. The co-precipitation temperature is varied in the range of $30-80^{\circ}C$. Calcination of the prepared precursors with $Li_2CO_3$ for 8 h at $1000^{\circ}C$ in air results in Li $Ni_{1/3}Co_{1/3}Mn_{1/3}O_2$ powders. Two kinds of obtained powders have been characterized by X-ray diffraction (XRD), scanning electron microscopy, particle size analyzer, and tap density measurements. The co-precipitation temperature does not differentiate the XRD patterns of precursors as well as their final powders. Precursor powders are spherical and dense, consisting of numerous acicular or flaky primary particles. The precursors obtained at 70 and $80^{\circ}C$ possess bigger primary particles having more irregular shapes than those at lower temperatures. This is related to the lower tap density measured for the former. The final powders show a similar tendency in terms of primary particle shape and tap density. Electrochemical characterization shows that the initial charge/discharge capacities and cycle life of final powders from the precursors obtained at 70 and $80^{\circ}C$ are inferior to those at $50^{\circ}C$. It is concluded that the optimum co-precipitation temperature is around $50^{\circ}C$.