• Journal of the Korean Electrochemical Society
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• v.20 no.4
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• pp.67-74
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• 2017

Layered Ni-rich NCM cathode materials $Li[Ni_xCo_{(1-x)/2}Mn_{(1-x)/2}]O_2$ ($x{\geq}0.6$) have advantages of high energy density and cost competitive over $LiCoO_2$. The discharge capacity of NCM increases proportionally to the Ni contents. However, there is a problem that it is difficult to realize the stable electrochemical performance due to cation mixing. In this study, synthesis conditions for the layered Ni-rich NCMs are investigated to achieve deliver the ones having good electrochemical performances. Synthesis parameters are atmosphere, lithium source, synthesis time, synthesis temperature and Li/M (M=transition metal) ratio. The degree of cation mixing gets worse as the Ni content is increased from $Li[Ni_{0.6}Co_{0.2}Mn_{0.2}]O_2$ (NCM6) to $Li[Ni_{0.8}Co_{0.1}Mn_{0.1}]O_2$ (NCM8). It is confirmed that higher level of cation mixing affects negatively on the electrochemical performance of NCMs. Optimum synthesis conditions are explored for NCMx (x=6, 7, 8) in order to reduce the cation mixing. Under optimized conditions for three representative NCMx, a high initial discharge capacity and a good cycle life are obtained for $180mAh{\cdot}g^{-1}$, 96.2% (50 cycle) in NCM6, $187mAh{\cdot}g^{-1}$, 94.7% (50 cycle) in NCM7, and $201mAh{\cdot}g^{-1}$, 92.7% (50 cycle) in NCM8, respectively.

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

• Economic and Environmental Geology
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• v.56 no.1
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• pp.23-53
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• 2023

In this review paper, previous studies on layered double hydroxides (LDHs) published in the Korean Citation Index (KCI) were examined to investigate a research trend for LDHs in Korea. Since the first publication in 2002, 160 papers on LDHs have been published until January 2023. Among the 31 academic fields, top 5 fields appeared in the order of chemical engineering, chemistry, materials engineering, environmental engineering, and physics. The chemical engineering shows the highest record of published paper (71 papers) while around 10 papers have been published in the other four fields. All papers were reclassified into 15 research fields based on the industrial and academic purposes of using LDHs. The top 5 in these fields are in order of environmental purification materials, polymer catalyst materials, battery materials, pharmaceutical/medicinal materials, and basic physicochemical properties. These findings suggest that researches on the applications of LDH materials in the academic fields of chemical engineering and chemistry for the improvement of their functions such as environmental purification materials, polymer catalysts, and batteries have been being most actively conducted. The application of LDHs for cosmetic and agricultural purposes and for developing environmental sensors is still at the beginning of research. Considering a market-potential and high-efficiency-eco-friendly trend, however, it will deserve our attention as emerging application fields in the future. All reclassified papers were summarized in our tables and a supplementary file, including information on applied materials, key results, characteristics and synthesis methods of LDHs used. We expect that our findings of overall trends in LDH research in Korea can help design future researches with LDHs and suggest policies for resources and energies as well as environments efficiently.

• Analytical Science and Technology
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• v.10 no.3
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• pp.209-215
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• 1997

Li-AGICs as a anode of secondary battery were synthesized by high-pressure method as a function of the Li-contents. The characteristics of these prepared compounds were determined from the studies with X-ray diffraction method, UV/VIS spectrophotometric and differential scanning calorimeter(DSC) analysis. From the results of X-ray diffraction, it was found that the lower stage intercalation compounds were formed with increase of Li-contents. The mixed stages in these compounds were also observed. In the case of the $Li_{30wt%}$-AGIC, the compounds in the stage 1 structure were formed predominantly, but the structure of only pure stage 1 for structural defect of artificial graphite is not observed. According to UV/VIS spectrophotometric analysis, $Li_{30wt%}$-AGIC shows distinguishable energy state spectrum with the position of $R(%)_{min}$ values, but the characteristic spectra of almost all Li-AGICs are not observed. The enthalpy and entropy changes of the compounds can be obtained from the differential scanning calorimetric analysis results. From the results, it was found that exothermic and endothermic reactions of Li-AGICs are related to thermal stability of lithium between artificial graphite layers.

• Journal of the Korean Electrochemical Society
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• v.21 no.3
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• pp.47-54
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• 2018

To maximize the areal capacity($mAh\;cm^{-2}$) of $LiNi_{0.5}Co_{0.2}Mn_{0.3}O_2$(NCM523) electrode with the same loading level of $15mg\;cm^{-2}$, three NCM523 electrodes with 4, 2, and 1 wt% poly(vinylidene fluoride)(PVdF) binder content are fabricated. Due to the delamination issue of electrode composite at the edge during punching process, the 1 wt% electrode is excluded for further evaluation. When the PVdF binder content decreases from 4 to 2 wt%, both adhesion strength and shear stress decrease from 0.4846 to $0.2627kN\;m^{-1}$ by -46% and from 3.847 to 2.013 MPa by -48%, respectively. Regardless of these substantial decline of mechanical properties, their initial electrochemical properties such as initial coulombic efficiency and voltage profile are almost the same. However, owing to high loading level, the 2 wt% electrode not only exhibits worse cycle performance than the 4 wt% electrode, but also cannot maintain its mechanical integrity only after 80 cycles. Therefore, if the binder content is reduced to increase the area capacity, the mechanical properties as well as the cycle performance must be carefully evaluated.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.25 no.5
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• pp.398-402
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• 2012

Synthesis of $Li_2MnSiO_4$ was attempted by the conventional solid-state reaction method, and the phase formation behavior according to the change of the calcination condition was investigated. When the mixture of the three source materials, $Li_2O$, MnO and $SiO_2$ powders, were used for calcination in air, it was difficult to develop the $Li_2MnSiO_4$ phase because the oxidation number of $Mn^{2+}$ could not be maintained. Therefore, two-step calcination was applied: $Li_2SiO_3$ was made from $Li_2O$ and $SiO_2$ at the first step, and $Li_2MnSiO_4$ was synthesized from $Li_2SiO_3$ and MnO at the second step. It was easy to make $Li_2MnSiO_3$ from $Li_2O$ and $SiO_2$. $Li_2MnSiO_4$ single phase was developed by the calcination at $900^{\circ}C$ for 24 hr in Ar atmosphere as the oxidation of $Mn^{2+}$ was prevented. However, the $Li_2MnSiO_4$ was ${\gamma}-Li_2MnSiO_4$, one of the polymorph of $Li_2MnSiO_4$, which could not be used as the cathode materials in Li-ion batteries. By applying the additional low temperature annealing at $400^{\circ}C$, the single phase ${\beta}-Li_2MnSiO_4$ powder was synthesized successfully through the phase transition from ${\gamma}$ to ${\beta}$ phase.

• Analytical Science and Technology
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• v.7 no.3
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• pp.315-320
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• 1994

Li-GICs as a high performance energy storager were synthesized as a function of the Li content by the admixture and add-pressure method. The characteristics of these prepared compounds have been determined from the studies by X-ray diffraction, UV-VIS spectrometry and CHN analysis. It follows from the results of X-ray diffraction that the lower-stage intercalation compounds are formed as the Li contents increase, however the mixed stages in these compounds are also observed. In the case of the $Li_{40wt%}$, the compound with the structure of stage 1 has been predominently, but the structure of only stage 1 is not obtained. The $d_{001}$ value of stage 1 was determined to be ca. $3.70{\AA}$. An analysis of spectrometric data shows that each of the compounds gives distingushible energy state spectra. It is seen from the spectra that the positions of $R_{min}$ values, with increase in the Li contents, are shifted in the region of higher energy state. Such a result can be attributed to the formation of stable stages. The results of CHN analysis allow us to find the mixing state related to chemical compositions of the intercalated compounds and the superiority to admixture and add-pressure method. From the results determined, it reveals that $Li_{10wt%}$-GIC and $Li_{20wt%}$-GIC can be utilized for an anode of rechargable battery.

• Korean journal of applied entomology
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• v.19 no.1 s.42
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• pp.5-9
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• 1980

Some insecticides were evaluated on the effect of single ULV foliar spray in the control of the pine gall midges (Thecediplosis japonensis Uchida et Inouye) when the formulated (undiluted) and/or diluted insecticides were applied by ULV Sprayer (Battery-type of 12 voltage, devised by Union Carbide) With the formulated insecticide spray (30ml per plot; ten pine trees of 1.5 to 2m in height), the order of control effectiveness was Salithion (Ec 25), $Sumithion^{(R)}$ (ULV 80), Dimethoate (Ec 50), $Sevin\;oil^{(R)}$ (ULV 50), $Zolone^{(R)}$ (Ec 25) and $Folimat^{(R)}$ (Ec 50). However, except Zolone, other insecticides tested caused relatively severe phytotoxicity on the pine needles in all treatments. The dilluted insecticides (200ml Per Plot) of Salithion and Dimethoate with 10,20 and 40 times of water solution showed better control effect than with the formulated insecticides, and no phytotoxicity was observed. Salithion was more effective than Dimethoate. In conclusion, the desirable results in the pine gall midge control in this experiment were obtained by single ULV foliar spray of Salithion with 10 to 20 times of water solution, and the feasible timing of insecticide application would be from late in May to early in June.

• Journal of the Korean Ceramic Society
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• v.56 no.2
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• pp.111-129
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• 2019

Recently, all-solid-state batteries (ASSBs) have attracted increasing interest owing to their higher energy density and safety. As the core material of ASSBs, the characteristics of the solid electrolyte largely determine the performance of the battery. Thus far, a variety of inorganic solid electrolytes have been studied, including the NASICON-type, LISICON-type, perovskite-type, garnet-type, glassy solid electrolyte, and so on. The garnet Li₇La₃Zr₂O₁₂ (LLZO) solid electrolyte is one of the most promising candidates because of its excellent comprehensively electrochemical performance. Both, experiments and theoretical calculations, show that cubic LLZO has high room-temperature ionic conductivity and good chemical stability while contacting with the lithium anode and most of the cathode materials. In this paper, the crystal structure, Li-ion transport mechanism, preparation method, and element doping of LLZO are introduced in detail based on the research progress in recent years. Then, the development prospects and challenges of LLZO as applied to ASSBs are discussed.

• Membrane Journal
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• v.27 no.5
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• pp.415-424
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• 2017

Commonly cation exchange membranes have been used for vanadium redox flow batteries. However, a severe vanadium ion cross-over causes low energy efficiency. Thus in this study, we prepared 3 different anion exchange membranes to investigate the effect on the membrane properties such as vanadium ion cross-over and long term stability. The base membranes were prepared by an electrolyte pore filling technique using vinyl benzyl chloride (VBC), divinylbenzene (DVB) within a porous polyethylene (PE) substrate. Then 3 different functional amines were introduced into the base membranes, respectively. These resulting membranes were evaluated by physico-chemical properties such as ion exchange capacity, dimensional stability, vanadium ion cross-over and membrane area resistance. Conclusively, TEA-functionalized membrane showed longest term stability than other membranes although all the membranes are similar to coulombic efficiency.