• 한국분말재료학회지
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• 제30권5호
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• pp.394-401
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• 2023

Li_1.5Al_0.5Ti_1.5(PO₄)₃ (LATP) is considered to be one of the promising solid-state electrolytes owing to its excellent chemical and thermal stability, wide potential range (~5.0 V), and high ionic conductivity (~10^-4 S/cm). LATP powders are typically prepared via the sol-gel method by adding and mixing nitrate or alkoxide precursors with chelating agents. Here, the thermal properties, crystallinity, density, particle size, and distribution of LATP powders based on chelating agents (citric acid, acetylacetone, EDTA) are compared to find the optimal conditions for densely sintered LATP with high purity. In addition, the three types of LATP powders are utilized to prepare sintered solid electrolytes and observe the microstructure changes during the sintering process. The pyrolysis onset temperature and crystallization temperature of the powder samples are in the order AC-LATP > CA-LATP > ED-LATP, and the LATP powder utilizing citric acid exhibits the highest purity, as no secondary phase other than LiTi₂PO₄ phase is observed. LATP with citric acid and acetylacetone has a value close to the theoretical density (2.8 g/cm³) after sintering. In comparison, LATP with EDTA has a low sintered density (2.2 g/cm³) because of the generation of many pores after sintering.

• 전기화학회지
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• 제18권2호
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• pp.45-50
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• 2015

본 연구에서는 리튬 이온 전도성 세라믹 고체전해질($Li_{1+x+y}Al_xTi_{2-x}Si_yP_{3-y}O_{12}$, LATP)의 알칼라인 용액 내에서의 화학적 안정성을 증가시키기 위하여, 고체전해질 표면을 질화 공정 처리를 통해 개질하였다. LATP 고체전해질의 화학적 안정성 및 전기화학 특성과 관련된 고체전해질 표면 형상 및 구조 특성 등을 X-선 회절법, X-선 광전자 분광법, 주사 전자 현미경 및 임피던스 측정을 통하여 분석하였다. 질화 처리된 LATP 시료를 30일간 알칼라인 용액에 담지하여, 표면 처리하지 않은 시료와 비교시 향상된 화학적 안정성을 나타냈으며, 이를 하이브리드 리튬-공기 전지에 적용하여 비교시 개선된 충방전 분극 및 효율 특성을 보였다. 이러한 결과를 바탕으로 질화 처리 공정을 통한 표면 개질은 알칼라인 용액내에서의 세라믹 고체전해질의 화학적 안정성을 증가시키는데 효과적으로 도움이 될 것으로 판단된다.

• 한국분말재료학회지
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• 제31권1호
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• pp.23-29
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• 2024

This study investigates the effect of the microstructure of Li_1.3Al_0.3Ti_1.7(PO₄)₃ (LATP), a solid electrolyte, on its ionic conductivity. Solid electrolytes, a key component in electrochemical energy storage devices such as batteries, differ from traditional liquid electrolytes by utilizing solid-state ionic conductors. LATP, characterized by its NASICON structure, facilitates rapid lithium-ion movement and exhibits relatively high ionic conductivity, chemical stability, and good electrochemical compatibility. In this study, the microstructure and ionic conductivity of LATP specimens sintered at 850, 900, and 950℃ for various sintering times are analyzed. The results indicate that the changes in the microstructure due to sintering temperature and time significantly affect ionic conductivity. Notably, the specimens sintered at 900℃ for 30 min exhibit high ionic conductivity. This study presents a method to optimize the ionic conductivity of LATP. Additionally, it underscores the need for a deeper understanding of the Li-ion diffusion mechanism and quantitative microstructure analysis.

• 한국분말재료학회지
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• 제30권2호
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• pp.107-115
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• 2023

Li_1.3Al_0.3Ti_1.7(PO₄)₃(LATP) is considered a promising material for all-solid-state lithium batteries owing to its high moisture stability, wide potential window (~6 V), and relatively high ion conductivity (10^-3-10^-4 S/cm). Solid electrolytes based on LATP are manufactured via sintering, using LATP powder as the starting material. The properties of the starting materials depend on the synthesis conditions, which affect the microstructure and ionic conductivity of the solid electrolytes. In this study, we synthesize the LATP powder using sol-gel and co-precipitation methods and characterize the physical properties of powder, such as size, shape, and crystallinity. In addition, we have prepared a disc-shaped LATP solid electrolyte using LATP powder as the starting material. In addition, X-ray diffraction, scanning electron microscopy, and electrochemical impedance spectroscopic measurements are conducted to analyze the grain size, microstructures, and ion conduction properties. These results indicate that the synthesis conditions of the powder are a crucial factor in creating microstructures and affecting the conduction properties of lithium ions in solid electrolytes.

• 한국전기전자재료학회논문지
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• 제36권6호
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• pp.627-632
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• 2023

Lithium-ion batteries are widely used in various applications, including electric vehicles and portable electronics, due to their high energy density and long cycle life. The performance of lithium-ion batteries can be improved by using solid electrolytes, in terms of higher safety, stability, and energy density. Li_1.5Al_0.5Ti_1.5(PO₄)₃ (LATP) is a promising solid electrolyte for all-solid-state lithium batteries due to its high ionic conductivity and excellent stability. However, the ionic conductivity of LATP needs to be improved for commercializing all-solid-state lithium battery systems. In this study, we investigate the microstructures and ionic conductivities of LATP by incorporating B₂O₃ glass ceramics. The smaller grain size and narrow size distribution were obtained after the introduction of B₂O₃ in LATP, which is attributed to the B₂O₃ glass on grain boundaries of LATP. Moreover, higher ionic conductivity can be obtained after B₂O₃ incorporation, where the optimal composition is 0.1 wt% B₂O₃ incorporated LATP and the ionic conductivity reaches 8.8×10^-5 S/cm, more than 3 times higher value than pristine LATP. More research could be followed for having higher ionic conductivity and density by optimizing the processing conditions. This facile approach for establishing higher ionic conductivity in LATP solid electrolytes could accelerate the commercialization of all-solid-state lithium batteries.

• 한국재료학회지
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• 제22권7호
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• pp.346-351
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• 2012

$Li_{1+x}Al_xTi_{2-x}(PO_4)_3$(LATP) is a promising solid electrolyte for all-solid-state Li ion batteries. In this study, LATP is prepared through a sol-gel method using relatively the inexpensive reagents $TiCl_4$. The thermal behavior, structural characteristics, fractured surface morphology, ion conductivity, and activation energy of the LATP sintered bodies are investigated by TG-DTA, X-ray diffraction, FE-SEM, and by an impedance method. A gelation powder was calcined at $500^{\circ}C$. A single crystalline phase of the $LiTi_2(PO_4)_3$(LTP) system was obtained at a calcination temperature above $650^{\circ}C$. The obtained powder was pelletized and sintered at $900^{\circ}C$ and $1000^{\circ}C$. The LTP sintered at $900{\sim}1000^{\circ}C$ for 6 h had a relatively low apparent density of 75~80%. The LATP(x = 0.3) pellet sintered at $900^{\circ}C$ for 6 h was denser than those sintered under other conditions and showed the highest ion conductivity of $4.50{\times}10^{-5}$ S/cm at room temperature. However, the ion conductivity of LATP (x = 0.3) sintered at $1000^{\circ}C$ decreased to $1.81{\times}10^{-5}$ S/cm, leading to Li volatilization and abnormal grain growth. For LATP sintered at $900^{\circ}C$ for 6 h, x = 0.3 shows the lowest activation energy of 0.42 eV in the temperature range of room temperature to $300^{\circ}C$.

• 전기화학회지
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• 제24권4호
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• pp.100-105
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• 2021

최근 리튬이차전지의 안전성을 향상시킨 전고체 전지가 많은 관심의 대상이 되고 있으나 전도성 세라믹 또는 고체 고분자 전해질을 적용한 고체전지는 높은 계면 저항, 부반응 등과 같은 문제점을 지니고 있어 전기화학적 특성이 낮다. 기존 전고체 전지의 이러한 문제점을 해결하기 위하여 복합고체 전해질이 제안되었으며 본 연구에서는 나시콘 구조의 나노 입자 Li_1.5Al_0.5Ti_1.5P₃O₁₂ (LATP) 전도성 세라믹, PVdF-HFP, 카보네이티 기반 액체전해질을 복합화 하여 유사고체 전해질을 제작하였다. 이 복합고체 전해질은 5.6 V의 높은 전압 안전성을 가지며 리튬이온의 탈리-착리 테스트에서 리튬 금속전극의 덴드라이트 성장 억제 효과가 있음을 보여준다. 또한 복합고체 전해질을 적용한 LiNi_0.83Co_0.11Mn_0.06O₂ (NCM811)기반 전지에서 4.8 V의 높은 충전 종지 전압에도 241.5 mAh/g의 높은 방전 용량을 나타내며 안정적인 전기화학 반응이 일어난다. NCM811 기반 전지의 90도 충전-방전 중에도 전지의 단락이나 폭발 없이 139.4 mAh/g 방전 용량을 보인다. 따라서 LATP기반 복합고체 전해질은 리튬이차전지의 안전성과 전기화학적 특성을 향상 시킬 수 있는 효과적인 방법임을 알 수 있다.

• 대한수학회지
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• 제46권6호
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• pp.1179-1192
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• 2009

In this note we give a new generalization of the notions of $Pr{\ddot{U}}fer$ domain and PvMD which uses quasi semistar invertibility, the "quasi P$\star$MD", and compare them with the P$\star$MD. We show in particular that the problem of when a quasi P$\star$MD is a P$\star$MD is strictly related to the problem of the descent to subrings of the P$\star$MD property and we give necessary and sufficient conditions.