• Korean Chemical Engineering Research
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• v.61 no.1
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• pp.39-44
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• 2023

In this study, the particle size of Si polycrystals was controlled through wet-sedimentation method, and changes in the capacity and cyclic characteristics of the Si anode material according to the particle size were observed. After wet-sedimentation of Si particles pulverized by a vibration mill, the non-uniform particle distribution of Si was uniformly controlled. The d₅₀ of a sample in which Si was sedimented for 24 hours decreased to 0.50 ㎛. As a result of the electrochemical characteristic analysis, the Rct value representing the resistance in the electrode was significantly reduced due to the decrease in particle size. The unclassified Si sample exhibited a discharge capacity of 2,869 mAh/g in the first cycle, and decreased to 85.7 mAh/g after 100 cycles. The sample in which Si was classified for 24 hours showed a capacity of 3,394 mAh/g initially, and maintained a capacity of 1,726 mAh/g after 100 cycles. As the size of the Si particles decreased, the discharge capacity increased and the cycle life was also increased.

• Clean Technology
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• v.14 no.3
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• pp.171-175
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• 2008

The effect of the addition of $Al^{3+}$ dopant on the electrochemical characteristics of $Li_{4}Ti_{5}O_{12}$ was investigated. $Li_{4}Ti_{5}O_{12}$ is known as a 2ero-strain material, and $Li_{3.95}Al_{0.15}Ti_{4.9}O_{12}$ has been manufactured by solid-state reaction with high energy ball milling (HEBM). The samples were heated at 800, 900 and $1000^{\circ}C$ in electric furnace. The structural and surface structures were measured by XRD (X-ray diffraction) and SEM (scanning electron microscopy). Cut-off voltage of charge/discharge cycles was $1.0{\sim}3.0 V$ to investigate reversible capacity, cycle stability and plateau voltage. The reversible capacity of $Li_{3.95}Al_{0.15}Ti_{4.9}O_{12}$ was 138 mAh/g.

• Korean Chemical Engineering Research
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• v.60 no.3
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• pp.327-333
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• 2022

In this study, silicon/carbon nanotube/carbon (Si/CNT/C) composites for anode were prepared to improve the volume expansion of silicon used as a high-capacity anode material. Si/CNT were prepared by electrostatic attraction of the positively charged Si and negatively charged CNT and then hydrothermal synthesis was performed to obtain the spherical Si/CNT/C composites. Poly(vinylidene fluoride) (PVDF), polyacrylic acid (PAA), and styrene butadiene rubber (SBR) were used as binders for electrode preparation, and coin cell was assembled using 1.0 M LiPF₆ (EC:DMC:EMC = 1:1:1 vol%) electrolyte and fluoroethylene carbonate (FEC) additive. The physical properties of Si/CNT/C anode materials were analyzed using SEM, EDS, XRD and TGA, and the electrochemical performances of lithium-ion batteries were investigated by charge-discharge cycle, rate performance, dQ/dV and electrochemical impedance spectroscopy tests. Also, it was confirmed that both capacity and rate performance were significantly improved using the PAA/SBR binder and 10 wt% FEC-added electrolyte. It is found that Si/CNT/C have the reversible capacity of 914 mAh/g, the capacity retention ratio of 83% during 50 cycles and the rate performance of 70% in 2 C/0.1 C.

• Korean Chemical Engineering Research
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• v.62 no.1
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• pp.19-26
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• 2024

In this study, the electrochemical properties of SiOx@C composite materials were prepared to alleviate volume expansion and cycle stability of silicon and to increase the capacity of anode material for LIBs. SiO₂ particles of 100, 200, and 500 nm were synthesized by the Stӧber method, and reduced to SiOx (0≤x≤2) through the magnesiothermic reduction method. Then, SiOx@C anode materials were synthesized by carbonization of PVC on SiOx. The physical properties of prepared SiOx and SiOx@C anode materials were analyzed by XRD, SEM, TGA, Raman spectroscopy, XPS and BET. The electrochemical properties were investigated by cycling performance, rate performance, CV and EIS test. As a result, the SiOx@C-7030 manufactured by coating carbon at SiOx : C = 70 : 30 on a 100 nm SiOx with the smallest particle size showed the best electrochemical properties with a discharge capacity of 1055 mAh/g and a capacity retention rate of 81.9% at 100 cycles. It was confirmed that cycle stability was impoved by reducing particle size and carbon coating.

• Korean Chemical Engineering Research
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• v.59 no.4
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• pp.487-492
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• 2021

In this study, the electrochemical properties of pitch coated silicon sheets/graphite anode materials were investigated. Using NaCl as a template, silicon sheets were prepared through the stöber method and the magnesiothermic reduction methode. In order to synthesize the anode composite, the silicon sheets and graphite were combined with SDBS. The pitch coated silicon sheets/graphite was synthesized using THF as a solvent for the anode material composite. The physical properties of the prepared anode composites were analysed by XRD, SEM, EDS and TGA. The electrochemical performances of the prepared anode composites were performed by the current charge/discharge, rate performance, cyclic voltammetry and EIS tests in the electrolyte LiPF₆ dissolved solvents (EC:DMC:EMC=1:1:1 vol%). As the silicon composition of silicon sheets/graphite composite material increased, the discharge capacity also increased, but the cycle stability tended to decrease. The anode material of pitch coated silicon sheets/graphite composite (silicon sheets:graphite=3:7 weight ratio) showed the initial discharge capacity of 1228.8 mAh/g and the capacity retention ratio of 77% after 50 cycles. From these results, it was found that the cycle stability of pitch coated silicon sheets/graphite was improved.

• Journal of the Korean Electrochemical Society
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• v.16 no.2
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• pp.59-64
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• 2013

Using $Na_2CO_3$ and $MeSO_4$ (Me = Ni, Co and Mn) as starting materials, the precursor of $[Ni_{0.6}Co_{0.2}Mn_{0.2}]CO_3$ has been synthesized by carbonate co-precipitation. The precursor was mixed with $Li_2CO_3$, and calcined at 750, 850, and$950^{\circ}C$ in air. Effect of calcinations temperature on characteristics of $Li[Ni_{0.6}Co_{0.2}Mn_{0.2}]O_2$ cathode materials was investigated. The structure and characteristics of $Li[Ni_{0.6}Co_{0.2}Mn_{0.2}]O_2$ were determined by X-ray diffraction (XRD), Scanning electron microscopy (SEM) and electrochemical measurements. The X-ray diffraction (XRD) results show that the intensity ratio of $I_{(003)}/I_{(104)}$ increased and the R-factor ratio decreased with the increase of calcinations temperature. And Scanning electron microscopy (SEM) result show that the primary particle size increased. Especially, the $Li[Ni_{0.6}Co_{0.2}Mn_{0.2}]O_2$ calcined at $950^{\circ}C$ for 24 H shows excellent electrochemical performances with reversible specific capacity of $165.3mAhg^{-1}$ [cut-off voltage 2.5~4.3 V, 0.1 C($17mAhg^{-1}$)] and good capacity retention of 95.4% after 50th charge/discharge cycles[cut-off voltage 2.5~4.3 V, 1 C($170mAhg^{-1}$)].

• Korean Chemical Engineering Research
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• v.57 no.6
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• pp.861-867
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• 2019

$Li_4Ti_5O_{12}$ is a promising next-generation anode material for lithium-ion batteries due to excellent cycle life, low irreversible capacity, and little volume expansion during charge-discharge process. However, it has poor charge capacity at high current density due to its low electrical conductivity. To improve this weakness, porous $Li_4Ti_5O_{12}$ was synthesized by sol-gel method with P123 as chelating agent. The physical characteristics of as-prepared sample was investigated by XRD, SEM, and BET analysis, and electrochemical properties were characterized by cycle performance test, cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS). $Li_4Ti_5O_{12}$ synthesized by 0.01mol ratio of P123/Ti showed most unified particle size, high specific surface area, and relatively high porosity. EIS analysis showed that depressed semicircle size was remarkably reduced, which suggested resistance value in electrode was decreased. Capacity in rate performance showed 178 mAh/g at 0.2C, 170 mAh/g at 0.5C, 110 mA/h at 5C, and 90 mAh/g at 10C. Capacity retention also showed 99% after rate performance.

• Korean Chemical Engineering Research
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• v.59 no.1
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• pp.42-48
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• 2021

Zn and Al added LiNi0.85Co0.15O2 cathode materials were synthesized to improve electrochemical properties and thermal stability using a solid-state route. Crystal structure, particle size and surface shape of the synthesized cathode materials was measured using XRD (X-ray diffraction) and SEM (scanning electron microscopy). CV (cyclic voltammetry), first charge-discharge profiles, rate capability, and cycle life were measured using battery cycler (Maccor, series 4000). Strong binding energy of Al-O bond enhanced structure stability of cathode material. Electrochemical properties were improved by preventing cation mixing between Li+ and Ni2+. Large ion radius of Zn+ increased lattice parameter of NC cathode material, which meant unit-cell volume was expanded. NCZA25 showed 80% of capacity retention at 0.5 C-rate during 100 cycles, which was 12% higher than that of NC cathode. The discharge capacity of NCZA25 showed 104 mAh/g at 5 C-rate. NCZA25 achieved 36 mAh/g more capacity than that of NC cathod. NCZA25 cathode material showed excellent rate capability and cycling performance.

• Clean Technology
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• v.24 no.1
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• pp.77-84
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• 2018

In this study, $Li_4Ti_5O_{12}$ anode materials for lithium ion battery were synthesized by dry ball-mill method. Polyvinyl chloride (PVC) as a carbon source was added to improve electrochemical properties. When the PVC was added after $Li_4Ti_5O_{12}$ formation, the spinel structure was well synthesized and it was confirmed by X-ray diffraction (XRD) experiments. When the carbon material was added before the synthesis and the heat treatment was performed, it was confirmed that a material having a different crystal structure was synthesized even when a small amount of carbon material was added. In the case of $Li_4Ti_5O_{12}$ without the carbon material, the electrical conductivity value was about $10{\mu}S\;m^{-1}$, which was very small and similar to that of the nonconductor. As the carbon was added, the electrical conductivity was greatly improved and increased up to 10,000 times. Electrochemical impedance spectroscopy (EIS) analysis showed that the size of semicircle corresponding to the resistance decreased with the carbon addition. This indicates that the resistance inside the electrode is reduced. According to the Cyclic voltammetry (CV) analysis, the potential difference between the oxidation peak and the reduction peak was reduced with carbon addition. This means that the rate of lithium ion insertion and deinsertion was increased. $Li_4Ti_5O_{12}$ with 9.5 wt% PVC added sample showed the best properties in rate capabilities of $180mA\;h\;g^{-1}$ at 0.2 C-rate, $165mA\;h\;g^{-1}$ at 0.5 C-rate, and $95.8mA\;h\;g^{-1}$ at 5 C-rate.