• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2004.07a
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• pp.134-137
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• 2004

새로운 리튬 2차전지용 양극활물질인 Li[NiMnCo]O2를 간단히 합성할 수 있는 방법과 Si의 doping에 의해 그 특성을 향상하였다. 원하는 당량비의 Li, Ni, Co, Mn의 nitrate를 고순도의 에탄올에 용해하고 여기에 Si의 원료물질로서 poly(methyl phenyl siloxane)을 원하는 양(전체 전이금속 이온의 $2{\sim}10\;mol%$)만큼 첨가한 후 약 30분 정도 교반하였다. 이 용액을 약 $70{\sim}80^{\circ}C$ 정도의 온도에서 고점도의 진흙 상태가 될 정도로 가열하고 $450{\sim}500^{\circ}C$의 온도에서 약 5시간 정도 열처리 하여 유기물이 없는 상태의 전구체를 제조하였다. 이 전구체를 분말형태로 분쇄하고 $600{\sim}650^{\circ}C$ 정도의 온도에서 3시간, $900{\sim}950^{\circ}C$ 정도의 온도에서 5시간 연속적으로 열처리 하여 최종 활물질을 제조하였다. 이렇게 제조된 활물질은 175mAh/g 정도의 높은 비용량을 나타내었으며 4.5V 충전 조건에도 우수한 수명특성을 나타내었다. Si이 doping되지 않은 활물질에 비해 Si이 doping된 물질은 율특성, 수명특성에서 보다 우수한 특성을 나타내었는데 이것은 층상구조 활물질의 격자상수 증가와 impedance 증가 억제에 기인한 것으로 분석되었다.

• Journal of the Korean Electrochemical Society
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• v.16 no.3
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• pp.151-156
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• 2013

As the cathode material for li-ion battery, $LiNi_{0.5}Mn_{0.3}Co_{0.2}O_2$ were synthesized by supercritical hydrothermal method and calcined $850^{\circ}C$ and $900^{\circ}C$ for 10hrs in air. The effect of temperature in the heat treatment on the powder and its performance were studied of xray diffraction pattern, SEM-image, physical properties and electrochemical behaviors. As a result, calcined at $900^{\circ}C$ material particle size more increase than calcined at $850^{\circ}C$ material, especially shows excellent electrochemical performance with initial reversible specific capacity of 163.84 mAh/g (0.1C/2.0-4.3V), 186.87 mAh/g (0.1C/2.0-4.5V) and good capacity retention of 91.49% (0.2C/2.0-4.3V) and 90.36% (0.2C/2.0-4.5V) after 50th charge/discharge cycle.

• Journal of the Korean Physical Society
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• v.73 no.10
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• pp.1535-1540
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• 2018

In this study, we prepared and characterized Nb-doped $Li_7La_3Zr_{2-x}O_{12}$ (LLZNO) powder and pellets with a cubic garnet structure by using a modified sol-gel synthesis and hot pressing. LLZNO powder with a very small grain size and cubic structure without secondary phases could be obtained by using a synthesis method in which Li and La sources in a propanol solvent were mixed together with Zr and Nb sources in 2-methoxy ethanol. A pure cubic phase LLZNO pellet could be fabricated from the prepared LLZNO and an additional 6-wt% of $Li_2CO_3$ powder by hot pressing at $1050^{\circ}C$ and 15.8 MPa. The hot-pressed LLZNO pellet with a relative density of 99% exhibited a very dense surface morphology. The total Li ionic conductivity of the hot-pressed LLZNO was $7.4{\times}10^{-4}S/cm$ at room temperature, which is very high level compared to other reported values. The activation energy for ionic conduction was estimated to be 0.40 eV.

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

• Applied Chemistry for Engineering
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• v.9 no.2
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• pp.220-225
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• 1998

The spinel structured $LiMn_2O_4$ was prepared from $Li_2CO_3$ and $MnO_2$ by calcination at various temperatures in the range of $750{\sim}900^{\circ}C$. It was found that the most suitable cubic structure of $LiMn_2O_4$ was obtained by heating at $850^{\circ}C$ for 12 hrs. However, in the calcination at $900^{\circ}C$, $Mn^{4+}$ of 0.06M was changed to $Mn^{+3}$ by the oxygen loss, so that it has been shown that the formula has changed to $LiMn_2O_{3.97}$. This phenomena were in agreement with the Jahn-Teller distortion by the increment of $Mn^{+3}$ ion on the octahedral sites of the spinel structured $LiMn_2O_4$. The results showed that after 15 charge/discharge cycles in the voltage range from 3.5V to 4.3V versus Li/$Li^+$ with a current density of $0.25mA/cm^2$, the spinel structured $LiMn_2O_4$ that was prepared at $900^{\circ}C$ showed a lower discharge capacity, 82~50 mAh/g, while the $LiMn_2O_4$, prepared at $850^{\circ}C$, showed the discharge capacity of 102~64 mAh/g.

• Journal of the Korean Electrochemical Society
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• v.2 no.1
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• pp.5-12
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• 1999

By the PVA-precursor method, polycrystalline powder of $Li_xNi_{1-y}Co_yO_2$, cathode material for lithium battery, was synthesized. Using the powder as the cathode material, lithium ion batteries were fabricated, whose electrochemical properties were measured. The effect of changing synthetic conditions, such as PvA/metal mole ratio, concentration of PVA, degree of polymerization of PVA, pyrolysis condition, and metal stoichiometry, on the battery performance was investigated. Considering the initial performance of the cell, the optimum stoichiometry of the $Li_xNi_{1-y}Co_yO_2$, synthesized by the PVA-precursor method was observed to be x: 1.0 and y=0.26. A minor phase of $Li_2CO_3$, which was generated by the residual carbon in the powder precursor, deteriorated the performance of the cell. In order to eliminate the minor phase, the precursor had to be pyrolyzed under the flow of dry air. Annealing the powder at $500^{\circ}C$ under the flow of dry air also eliminated the minor phase, and the performance of the cell was largely improved by the treatment.

• Journal of Electrochemical Science and Technology
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• v.14 no.3
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• pp.293-300
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• 2023

The global energy storage markets have gravitated to high-energy-density and low cost of lithium-ion batteries (LIBs) as the predominant system for energy storage such as electric vehicles (EVs). High-Ni layered oxides are considered promising next-generation cathode materials for LIBs owing to their significant advantages in terms of high energy density. However, the practical application of high-Ni cathodes remains challenging, because of their structural and surface instability. Although extensive studies have been conducted to mitigate these inherent instabilities, a two-step process involving the synthesis of the cathode and a dry/wet coating is essential. This study evaluates a one-step β-Li₂SnO₃ layer coating on the surface of LiNi_0.8Co_0.2O₂ (NC82) via the thermal segregation of Sn owing to the solubility limit with respect to the synthesis temperature. The doping, segregation, and phase transition of Sn were systematically revealed by structural analyses. Moreover, surface-engineered 5 mol% Sn-coated LiNi_0.8Co_0.2O₂ (NC82_Sn5%) exhibited superior capacity retention compared to bare NC82 owing to the stable surface coating layer. Thus, the developed one-step coating method is suitable for improving the properties of high-Ni layered oxide cathode materials for application in LIBs.

• Journal of the Korean Electrochemical Society
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• v.19 no.3
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• pp.63-68
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• 2016

$Li_4Ti_5O_{12}$ is prepared through a solid-state reaction between anatase $TiO_2$ and $Li_2CO_3$ for the negative electrode active materials in quick-charging lithium-ion batteries. The small amount of carbon black (0, 0.5, 1.0, and 3.0 wt%) is added for the reduction of powder agglomeration during heat-treatment. As the amount of the added carbon black increases, the tap density of $Li_4Ti_5O_{12}$ powder gradually decreases. Furthermore, the $Li_4Ti_5O_{12}$ powder prepared with 1.0 wt% of carbon black shows the highest sieved fraction at the powder classification by 325 mesh standard sieve. The $Li_4Ti_5O_{12}$ powders with various contents of carbon black are almost same at the rate capability for the negative electrode materials in lithium-ion batteries.

• Journal of Electrochemical Science and Technology
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• v.15 no.1
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• pp.168-177
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• 2024

Ni-rich cathode is one of the promising candidates for high-energy lithium-ion battery applications. Due to its specific capacity, easy industrialization, and good circulation ability, Ni-rich cathode materials have been widely used for lithium-ion batteries. However, due to the limitation of the co-precipitation method, including sewage pollution, and the instability of the long production cycles, developing a new efficient and environmentally friendly synthetic approach is critical. In this study, the Ni_0.91Co_0.06Mn_0.03CO₃ precursor powder was successfully synthesized by an efficient spray-drying method using carbonate compounds as a raw material. This Ni_0.91Co_0.06Mn_0.03CO₃ precursor was calcined by mixing with LiOH·H₂O (5 wt% excess) at 480℃ for 5 hours and then sintered at two different temperatures (780℃/800℃) for 15 hours under an oxygen atmosphere to complete the cathode active material preparation, which is a key component of lithium-ion batteries. As a result, LiNi_0.91Co_0.06Mn_0.03O₂ cathode active material powders were obtained successfully via a simple sintering process on the Ni_0.91Co_0.06Mn_0.03CO₃ precursor powder. Furthermore, the obtained LiNi_0.91Co_0.06Mn_0.03O₂ cathode active material powders were characterized. Overall, the material sintered at 780℃ shows superior electrochemical performance by delivering a discharge capacity of 190.76 mAh/g at 1^st cycle (0.1 C) and excellent capacity retention of 66.80% even after 50 cycles.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2007.11a
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• pp.259-259
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• 2007

층상구조의 전이금속 산화물($LiMO_2$, M=Co, Ni, Mn)은 리튬이차전지용 양극재료로 활발한 연구가 진행되고 있다. 차세대 리튬이차전지 시스템의 개발 및 고성능화를 위해서는 전지의 용량을 결정하는 핵심 부품인 양극재료의 고용량화 및 고안정화는 필수 불가결하다. 따라서 본 연구에서는 상업적으로 큰 장점이 있는 고상반응 공정을 이용하여 리튬이차전지용 양극소재를 제조하고, 소재의 전기화학적, 구조적인 특성을 평가하였으며, 다음과 같은 주제를 가지고 연구를 진행하였다. $LiCoO_2$ 양극재료는 리튬이온전지로 널리 사용되고 있다. 높은 에너지 밀도의 리튬이온전지를 얻기 위해서는 $LiCoO_2$ 양극재료가 고용량화 및 고밀도화를 가져야 한다. 여기서 $LiCoO_2$ 분말이 irregular particle morphology를 가지면 tap density가 $2.2-2.4gcm^{-3}$로 에너지 밀도가 낮으나, 구형 $LiCoO_2$의 정극재료는 tap density가 $2.6-2.8gcm^{-3}$로 상대적으로 energy density가 높아지는 효과가 있다. 구형 $LiCoO_2$ 양극재료를 합성하기 위해서는 chelating agent를 이용한 "controlled crystallization" 침전법을 사용하여 합성한 구형 코발트 수화물을 사용하고 있다. "controlled crystallization" 침전법에서 사용되는 chelating agent로는 주로 ammonia가 이용되고 있다. 본 연구에서는 chelating agent로 ethylene diamine을 사용하여 sodium hydroxides를 precipitation으로 침전 반응하여 구형 코발트 수화물을 합성하였다. 상기 방법으로 합성된 코발트 수화물과 리튬 수화물($LiOH{\cdot}H_2O$-고순도화학(高殉道化學))을 사용하여 고상법을 통하여 $LiCoO_2$를 합성하였다. 제조된 분말의 결정구조와 전기화학적 특성분석은 X-선 회절분석 및 리트벨트 구조정산, 그리고 충/방전 싸이클링을 수행하였으며, 분말의 미세구조 변화를 SEM을 이용하여 분석하였다.