• Journal of Powder Materials
• /
• v.23 no.4
• /
• pp.287-296
• /
• 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 $50^{\circ}C$.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
• /
• 2002.11a
• /
• pp.210-215
• /
• 2002

This thesis is contents on the crystal grown by the solide phase method at $925^{\circ}C$ with orthorhombic structure that $LiMnO_{2}$ active material synthesised with precurse $Mn_{2}O_{3}$ and $LiOH.H_{2}O$ material to get three voltage level. The porosity analysis of the grown crystal in secondary batteries $LiMnO_{2}$ thin film is $1.323E+02\AA$ of the average pore diameter of powder particles and its structure to be taken the pore diameter was prepared. Adding voltage area to get properties of charge and discharge of which experiment result of $LiMnO_{2}$ thin film area 2.2V~4.3V, current and scan speed were 0.1mAh/g and $0.2mV/cm^{2}$ respectively, and properties of the charge and discharge to be got optimum experiment condition parameter and density rate of Li for analyze that unit discharge capacity with metal properties is 87mAh/g was 96.9[ppm] at 670.784[nm] wavelength, and density rate of Mn analyzed 837[ppm] at 257.610[nm]. It can be estimated the quality of thin film that wrong cell reject from the bottle of electrolyte. The results of SEM and XRD were the same that of original researchers.

• Journal of the Korean Electrochemical Society
• /
• v.16 no.2
• /
• pp.59-64
• /
• 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($170mAhg^{-1}$)].

• Journal of the Korean Electrochemical Society
• /
• v.15 no.3
• /
• pp.172-180
• /
• 2012

The $LiMn_2O_4$ cathodes for lithium ion battery were synthesized from various precursors of manganese oxides and manganese hydroxides. As the first step, nanosized precursors such as ${\alpha}-MnO_2$ (nano-sticks), ${\beta}-MnO_2$ (nano-rods), $Mn_3O_4$ (nano-octahedra), amorphous $MnO_2$(nano-spheres), and $Mn(OH)_2$ (nano-plates) were prepared by a hydrothermal or a precipitation method. Spinel $LiMn_2O_4$ with various sizes and shapes were finally synthesized by a solid-state reaction method from the manganese precursors and LiOH. Nano-sized (500 nm) octahedron $LiMn_2O_4$ showed high capacities of 107 mAh $g^{-1}$ and 99 mAh $g^{-1}$ at 1 C- and 50 C-rate, respectively. Three dimensional octahedral crystallites exhibit superior electrochemical characteristics to the other one-dimensional and two-dimensional shaped $LiMn_2O_4$ nanoparticles. After 500 consecutive charge discharge battery cycles at 10 C-rate with the nano-octahedron $LiMn_2O_4$ cathode, the capacity retention of 95% was observed, which is far better than any other morphologies studied in this work.

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

• 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.

• 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.

• Journal of the Korean Electrochemical Society
• /
• v.10 no.1
• /
• pp.48-51
• /
• 2007

In order to investigate the effects of particle size and specific surface area(BET area) of spinel powder, $LiMn_2O_4$ were synthesized using metal oxide precursor by co-precipitation method(CoP) and solid state reaction (SSR) .X-ray diffraction(XRD) patterns revealed that the both prepared powder has a well developed spinel structure with Fd3m space group. The $LiMn_2O_4$ prepared by co-precipitation showed spherical morphology with narrow size distribution. However, the $LiMn_2O_4$ prepared by solid state reaction showed relatively smaller particles with irregular shape. The measured BET areas of the powers are $0.8m^2g^{-1}$ (CoP) and $3.6m^2g^{-1}$(SSR). The electrochemical performance of the Prepared $LiMn_2O_4$ powders was evaluated using coin type cells(CR2032) at elevated temperature ($55^{\circ}C$). The $LiMn_2O_4$ prepared by co-precipitation showed the better cycling performance(82.3%capacity retention at $50^{th}$ cycle) than that of the $LiMn_2O_4$(68.3%) prepared by solid state reaction at elevated temperature.

• Journal of the Korean Electrochemical Society
• /
• v.16 no.3
• /
• pp.162-168
• /
• 2013

$Li_2MnO_3-LiMO_2$(M=Ni, Co, Mn) nano-composite is a promising cathode material for xEV application due to its high theoretic capacity. However high voltage operating system of $Li_2MnO_3-LiMO_2$(M=Ni, Co, Mn) has worked as a hurdle in its application because of the inherent demerits, such as cycle life degradation and gas evolution. In order to enhance cell performance of $Li_2MnO_3-LiMO_2$(M=Ni, Co, Mn)/graphite cell, we examined electrolyte mainly composed of FEC, fluroalkyl ether and $LiPF_6$ (F-based EL). F-based EL showed much better discharging retention ratio than 1.3 M $LiPF_6$ EC/EMC/DMC (3/4/3, v/v/v) (STD). Furthermore gas evolution, especially CO and $CO_2$ during $60^{\circ}C$ storage for 30 days was dramatically reduced owing to thermal stable SEI formation effect of F-based EL.

• 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.