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권민재,한현일,신슬기,구상모,신원호,Min-Jae Kwon,Hyeon Il Han,Seulgi Shin,Sang-Mo Koo,Weon Ho Shin 한국전기전자재료학회 2023 전기전자재료학회논문지 Vol.36 No.6
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<sub>1.5</sub>Al<sub>0.5</sub>Ti<sub>1.5</sub>(PO<sub>4</sub>)<sub>3</sub> (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 B<sub>2</sub>O<sub>3</sub> glass ceramics. The smaller grain size and narrow size distribution were obtained after the introduction of B<sub>2</sub>O<sub>3</sub> in LATP, which is attributed to the B<sub>2</sub>O<sub>3</sub> glass on grain boundaries of LATP. Moreover, higher ionic conductivity can be obtained after B<sub>2</sub>O<sub>3</sub> incorporation, where the optimal composition is 0.1 wt% B<sub>2</sub>O<sub>3</sub> incorporated LATP and the ionic conductivity reaches 8.8×10<sup>-5</sup> 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.
Li1.5Al0.5Ti1.5(PO4)3세라믹 고체전해질의 B2O3첨가에 따른 미세구조 및 이온전도도에 대한 연구
권민재,한현일,신슬기,구상모,신원호 한국전기전자재료학회 2023 전기전자재료학회논문지 Vol.36 No.6
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. Li1.5Al0.5Ti1.5(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.
Luhur Muhammad Sadewo Panghudi(루흐르 무하마드 사데오 팡후디),Geum-ji Jang(장금지),Kwang-Sun Ryu(류광선) 한국전지학회 2022 한국전지학회지 Vol.2 No.1
NASICON계 Li<SUB>1.3</SUB>Al<SUB>0.3</SUB>Ti<SUB>1.7</SUB>(PO₄)₃ (LATP) 산화물계 고체전해질은 양호한 기계적 물성, 높은 Li<SUP>+</SUP> 이동수, 우수한 전기화학적 및 열적 안정성을 나타낸다. LATP의 이온전도도를 높이기 위해 수용성 바인더를 도입하였다. 은은 개질된 고체 방법을 사용하여 Li<SUB>1.3</SUB>Al<SUB>0.3</SUB>Ti<SUB>1.7</SUB>(PO₄)₃ 고체 전해질에 성공적으로 치환되었다. Pristine Li<SUB>1.3</SUB>Al<SUB>0.3</SUB>Ti<SUB>1.7</SUB>(PO₄)₃ 도 치환 전 후를 비교하기 위해 합성되었다. X-ray 회절 패턴은 바인더의 첨가 후 피크의 이동을 보였으며 이는 전해질에 대한 바인더의 영향으로 나타났다. 은으로 개질된 Li<SUB>1.3</SUB>Al<SUB>0.3</SUB>Ti<SUB>1.7</SUB>(PO₄)₃에서 넓고 증가된 피크가 발견되었다. 또한 46.5° 부근에서 작은 새로운 피크가 나타났는데, 이는 LATP에 은이 성공적으로 치환되었음을 나타낸다. 이온전도도 측정은 EIS (Electrochemical Impedance Spectroscopy)로 수행되었으며 고체 전해질 용 바인더로서 1% PVA가 사용된 Li<SUB>1.3</SUB>Al<SUB>0.3</SUB>Ti<SUB>1.7</SUB>(PO₄)₃가 4.65 × 10<SUP>-5</SUP> S/cm의 가장 높은 값을 나타낸다. NASICON-type Li<SUB>1.3</SUB>Al<SUB>0.3</SUB>Ti<SUB>1.7</SUB>(PO₄)₃ (LATP) oxide-based solid electrolyte shows the favorable mechanical property, high Li+ transfer number, and excellent electrochemical and thermal stability. Water-soluble binders were introduced in order to increase the ionic conductivity of LATP. Silver was successfully substituted to the Li<SUB>1.3</SUB>Al<SUB>0.3</SUB>Ti<SUB>1.7</SUB>(PO₄)₃ solid electrolyte using a modified solid-state method for all-solid-state lithium batteries (ASSLBs). The pristine Li<SUB>1.3</SUB>Al<SUB>0.3</SUB>Ti<SUB>1.7</SUB>(PO₄)₃ was also synthesized for comparison before and after silver modification. X-ray diffraction patterns showed the peak shifting after the addition of binders were shown as the effect of binders on the electrolyte. A similar peak with slightly increased and peak broadening for silver-modified LATP appeared after the addition of silver. There are also a small new peak appeared at around 46.5° theta degree indicating that the modification of silver on LATP has successfully synthesized. The ionic conductivity measurement was conducted by Electrochemical Impedance Spectroscopy (EIS) and revealed LATP with 1% PVA is currently displaying a highest value of 4.65 × 10<SUP>-5</SUP> S/cm as binder for solid electrolytes.
LATP 내 비정상 입자성장이 이온 전도도에 미치는 영향
최형익,한윤수 한국분말재료학회(구 한국분말야금학회) 2024 한국분말재료학회지 (KPMI) Vol.31 No.1
This study investigates the effect of the microstructure of Li1.3Al0.3Ti1.7(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 950oC 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 900oC 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.
Sol-Gel법에 의한 Li1.5Al0.5Ti1.5(PO4)3 고체전해질 제조 및 chelating agent의 영향
류성준,최슬기,원종호,양민호 한국분말재료학회 2023 한국분말재료학회지 (KPMI) Vol.30 No.5
Li1.5Al0.5Ti1.5(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.
합성 방법에 따른 Li1.3Al0.3Ti1.7(PO4)3 소결체의 미세 구조 및 이온전도 특성 연구
최슬기,최재원,양민호 한국분말재료학회 2023 한국분말재료학회지 (KPMI) Vol.30 No.2
Li1.3Al0.3Ti1.7(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.
김주미,오지민,신동옥,김주영,이명주,이영기,김광만 한국공업화학회 2018 한국공업화학회 연구논문 초록집 Vol.2018 No.0
The composite polymer gel electrolytes(CPGE) for lithium-ion batteries are prepared by combining the binary polymer components of hydroxypropylcellulose (HPC), poly vinylidenefluoride-co-hexafluoropropylene (PVdF-HFP), the inorganic filler of Li<sub>1.3</sub>Al<sub>0.3</sub>Ti<sub>1.7</sub>(PO<sub>4</sub>)<sub>3</sub> (LATP) and the electrolyte solution of 1 M LiPF<sub>6</sub>/EC:PC:EMC. Three main solid components play their own roles in the composite electrolytes. The synergy among each component is expected to lead highly ionic conductive electrolytes with excellent mechanical strength. In this study, the effect of LATP content on the physical and electrochemical properties of the CPGE is particularly investigated. The LATP is used as powder obtained after the calcination at 900℃ and before pressing the hydrothermally synthesized product. In the presentation, how each component and its content contribute to the electrochemical performance of the cell will also be discussed in detail.
윤영섭,김정훈,박찬휘,신동욱 한양대학교 세라믹연구소 2013 Journal of Ceramic Processing Research Vol.14 No.4
Lithium ion conducting NASICON-type electrolytes of general formula Li1.3Al0.3Ti1.7(PO4)3 (LATP) are fabricated by a citric acid-supported sol-gel process and analyzed for thermal stability, microstructure, crystalline phases. From these structural analyses, the relationship of microstructural changes and electrochemical properties is investigated. It is demonstrated that the sol-gel method enable to obtain pure LATP crystals at a lower temperature in a shorter synthesis time compared to conventional solid state reaction or glass-ceramics processes. The dense electrolyte pellets are prepared from the LATP nanopowders by sintering at 900 o C for 3 hours, and a room temperature conductivity of 7.8 × 10-5S/cm and activation energy of 38.2 KJ/mol was obtained.