• Bulletin of the Korean Chemical Society
• /
• v.35 no.5
• /
• pp.1516-1522
• /
• 2014

A series of 20 wt % $(NH_4)_2SO_4$ and 3 wt % $Al_2O_3$ surface treatments were applied to $Li[Li_{0.2}Mn_{0.54}Co_{0.13}Ni_{0.13}]O_2$ substrates. The $Li[Li_{0.2}Mn_{0.54}Co_{0.13}Ni_{0.13}]O_2$ substrates were synthesized using a co-precipitation method. Sample (a) was left pristine and variations of the 20 wt % $(NH_4)_2SO_4$ and 3 wt % $Al_2O_3$ were applied to samples (b), (c) and (d). XRD was used to verify the space group of the samples as R$\bar{3}$m. Additional morphology and particle size data were obtained using SEM imagery. The $Al_2O_3$ coating layers of sample (b) and (d) were confirmed by TEM images and EDS mapping of the SEM images. 2032-type coin cells were fabricated in a glove box in order to investigate their electrochemical properties. The cells were charged and discharged at room temperature ($25^{\circ}C$) between 2.0V and 4.8V during the first cycle. The cells were then charged and discharged between 2.0V and 4.6V in subsequent cycles. Sample (d) exhibited lower irreversible capacity loss (ICL) in the first charge-discharge cycle as compared to sample (c). Sample (d) also had a higher discharge capacity of ~250 mAh/g during the first and second charge-discharge cycles when compared with sample (c). The rate capability of the $Al_2O_3$-coated sample (b) and (d) was lower when compared with sample (a) and (c). Sample (d), coated with $Al_2O_3$ after the surface treatment with $(NH_4)_2SO_4$, showed an improvement in cycle performance as well as an enhancement of discharge capacity. The thermal stability of sample (d) was higher than that of the sample (c) as the result of DSC.

• Korean Chemical Engineering Research
• /
• v.56 no.5
• /
• pp.718-724
• /
• 2018

In this study, the $Ni_{0.9}Co_{0.05}Ti_{0.05}(OH)_2$ precursor was prepared by the concentration gradient co-precipitation method. In order to overcome the structural change due to oxygen desorption in the cathode active material with high nickel content, the physical and electrochemical analysis of the cathode active material according to the calcination temperature were investigated. Physical properties of $Li_{1.05}Ni_{0.9}Co_{0.05}Ti_{0.05}O_2$ were analyzed by FE-SEM, XRD and TGA. The electrochemical performance of the coin cell using a cathode active material and $LiPF_6$(EC:EMC=1:2 vol%) electrolyte was evaluated by the initial charge/discharge efficiency, cycle retention, and rate capabilities. As a result, the initial capacity and initial efficiency of cathode materials were excellent with 244.5~247.9 mAh/g and 84.2~85.8% at the calcination temperature range of $750{\sim}760^{\circ}C$. Also, the capacity retention exhibited high stability of 97.8~99.1% after 50cycles.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
• /
• 2009.06a
• /
• pp.462-462
• /
• 2009

$CeO_2$는 고체 산화물 연료전지 (SOFC, soild oxide fuel cell)의 전해질 재료와 CMP(Chemical Mechanical Polishing) 슬러리 재료, 자동차의 3원 촉매, gas sensor, UV absorbent등 여러 분야에서 사용되고 있다. 본 연구에서는 위의 활용범위 외에 $CeO_2$의 구조적 안정성과 빠른 $Ce^{3+}/Ce^{4+}$의 전환 특성을 이용하여 lithium ion battery의 anode 재료로서 전기화학적 특성을 알아보고자 실험을 실시하였다. $CeO_2$ 합성에 사용되는 전구체인 cerium carbonate의 형상 및 크기, 비표면적과 같은 물리화학적 특성이 $CeO_2$ 분말의 특성에 직접적인 영향을 주기 때문에 전구체의 합성 단계에서 입자의 특성을 조절하였다. 전구체 합성의 출발원료로 cerium nitrate hexahydrate 와 ammonium carbonate를 사용하였고 반응온도 및 농도 등을 변화시켜 입자의 형상 및 결정상을 fiber형태의 orthorombic $Ce_2O(CO_3)_2{\cdot}H_2O$와 구형의 hexagonal $CeCO_3OH$의 세리아 전구체를 합성하였다. 이를 $300^{\circ}C$에서 30분 동안 하소하여 전구체의 입자형상을 유지하는 cubic $CeO_2$를 합성하고 X-ray diffraction, FE-SEM, micropore physisorption analyzer 분석을 통하여 입자의 결정상과 형상, 비표면적 등을 비교 분석하고 $Li/CeO_2$ couple의 충,방전 용량과 수명특성을 비교 분석하여 $CeO_2$의 전기화학적 특성을 알아보았다.

• Journal of the Korean Electrochemical Society
• /
• v.18 no.3
• /
• pp.130-135
• /
• 2015

The rate capability and low-temperature characteristics of graphite electrode are investigated after surface treatment with copper phthalocyanine (CuPc) or phthalocyanine (Pc). Uniform coating layers comprising amorphous carbon or copper are generated after the treatment. The rate performance of graphite electrodes is enhanced by the surface treatment, which is more prominent with CuPc. The resistance of the graphite electrode estimated from electrochemical impedance spectroscopy and pulse resistance measurement is the smallest for the CuPc-treated graphite. It is likely that the amorphous carbon layer formed by the decomposition of Pc facilitates $Li^+$ diffusion and the metallic copper derived from CuPc improves the electrical conductivity of the graphite electrode.

• Journal of the Korean Electrochemical Society
• /
• v.12 no.2
• /
• pp.189-195
• /
• 2009

$\beta-Ga_{2}O_{3}$ nanorods were synthesized by chemical vapor deposition method using nickel-oxide nanoparticle as a catalyst and gallium metal powder as a source material. The average diameter of nanorods was around 160 nm and the average length was $4{\mu}m$. Also, we confirmed that the synthesis of nanorods follows the vapor-solid growth mechanism. From the results of X-ray diffraction and HR-TEM observation, it can be found that the synthesized nanorods consisted of a typical core-shell structure with single-crystalline $\beta-Ga_{2}O_{3}$ core with a monoclinic crystal structure and an outer amorphous gallium oxide layer. Li/$\beta-Ga_{2}O_{3}$ nanorods cell delivered capacity of 867 mAh/g-$\beta-Ga_{2}O_{3}$ at first discharge. Although the Li/$\beta-Ga_{2}O_{3}$ nanorods cell showed low coulombic efficiency at first cycle, the cell exhibited stable cycle life property after fifth cycle.

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

• Korean Chemical Engineering Research
• /
• v.62 no.3
• /
• pp.246-252
• /
• 2024

In this study, impurities such as Li and F were removed from waste graphite through citric acid treatment, and changes in structural properties, capacity, and cycle stability of regenerated graphite were observed accordingly. Regenerated graphite pretreated in a nitrogen atmosphere was treated with citric acid, and its structure and characteristics were analyzed through SEM (Scanning Electron Microscope), FT-IR (Fourier Transform Infrared spectroscopy), XRD (X-ray Diffraction), and XPS (X-ray Photoelectron Spectroscopy). Waste graphite that was not treated with acid had a rapid decrease in capacity before 70 cycles, but graphite that had been treated with citric acid showed a capacity of 302.9 mAh g^-1 and a capacity retention rate of 93.1% at 100 cycles. In addition, despite changes in current density in rate performance, samples treated with citric acid showed 340.2 mAh g^-1 performance at 1.0C without change in capacity. As a result, it was confirmed that citric acid treatment not only effectively removed impurities and showed a high capacity retention rate, but also showed stability even at high current densities.

• Korean Chemical Engineering Research
• /
• v.62 no.3
• /
• pp.262-268
• /
• 2024

In this study, the MXene/Si composite was prepared by electrostacic assembly with 2-dimensional structured titanium carbide (MXene) and nano silicon for anode material of high-performance lithium-ion battery. Ti₃C₂T_x MXene was synthesized by etching the Ti₃AlC₂ MAX with LiF/HCl, and the surface of nano silicon was charged to positively using CTAB (Cetyltrimethylammonium bromide). The MXene/Si anode composite was successfully manufactured by simple mixing process of synthesized MXene and charged silicon. The physical and electrochemical properties of prepared composite were investigated with MXene-silicon composition ratio, and the surface of electrode after cycles was analyzed to evaluate stability of the electrode. The MXene/Si composites demonstrated high initial discharge capacities of 1962.9, 2395.2 and 2504.3 mAh/g as the silicon composition ratio increased to 2, 3 and 4 compared to MXene, respectively. MXene/Si-4, which is MXene and silicon ratio with 1 : 4, exhibited 1387.5 mAh/g of reversible capacity, 74.5% of capacity retention at 100 cycles and high capacity of 700.5 mAh/g at high rate of 4.0 C. As the results, the MXene/Si composite prepared by electrostatic-assenbly could be applied to anode materials for high-performance LIBs.

• Journal of the Korean Electrochemical Society
• /
• v.17 no.2
• /
• pp.111-118
• /
• 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 the Korean Electrochemical Society
• /
• v.24 no.4
• /
• pp.120-132
• /
• 2021

Although the development of high-Nickel is being actively carried out to solve the capacity limitation and the high price of raw cobalt due to the limitation of high voltage use of the existing LiCoO₂, the deterioration of the battery characteristics due to the decrease in structural stability and increase of the Ni content. It is an important cause of delaying commercialization. Therefore, in order to increase the high stability of the Ni-rich ternary cathod material LiNi_0.6Co_0.2Mn_0.2O₂, precursor Ni_0.6Co_0.2Mn_0.2-x(OH)₂/xTiO₂ was prepared using a nanosized TiO₂ suspension type source for uniform Ti substitution in the precursor. It was mixed with Li₂CO₃, and after heating, the cathode active material LiNi_0.6Co_0.2Mn_0.2-xTi_xO₂ was synthesized, and the physical properties according to the Ti content were compared. Through FE-SEM and EDS mapping analysis, it was confirmed that a positive electrode active material having a uniform particle size was prepared through Ti-substituted spherical precursor and Particle Size Analyzer and internal density and strength were increased, XRD structure analysis and ICP-MS quantitative analysis confirmed that the capacity was effectively maintained even when the Ti-substituted positive electrode active material was manufactured and charging and discharging were continued at high temperature and high voltage.