• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2007.11a
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• pp.316-316
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• 2007

리튬폴리머 전지용 정극활물질인 $LiFePO_4$를 수열법으로 합성하였다. 제조한 정극활물질 $LiFePO_4$는 X-ray 회절분석을 통하여 olivine 구조임을 확인하였다. 전극 제조 시 첨가된 도전재의 종류에 따른 전기화학적 특성변화를 알기 위하여, Acetylene Black, Super-Black, Multi-Walled Carbon Nanotube(MWCNT), SP270을 도전재로 제조된 정극활물질과 PVDF를 결합제로 사용하였다. 셀은 제조된 정극과 고체전해질 $25PVDFLiCIO_4EC_{10}PC_{10}$를 사용하고, 부극은 금속리튬으로 coin 타입의 cell을 조립하여 충방전을 진행하였다. 충방전 진행결과, Multi-Walled Carbon Nanotube(MWCNT)를 도전재로 사용하였을 경우, 초기 방전용량은 94mAh/g, 100cycle 후에는 약 93mAh/g인 기타 도전재를 사용하였을 때보다 안정하고 높은 방전용량을 나타내었다. 이때의 충방전 전류밀도는 0.1mAh/g이고 전압범위 는 2.5~4.3V이었다.

• Korean Journal of Materials Research
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• v.25 no.8
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• pp.423-428
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• 2015

Impedancemetric $NO_x$ (NO and $NO_2$) gas sensors were designed with a stacked-layer structure and fabricated using $LaCr_xCo_{1-x}O_3$ (x = 0, 0.2, 0.5, 0.8 and 1) as the receptor material and $Li_{1.3}Al_{0.3}Ti_{1.7}(PO_4)_3$ plates as the solid-electrolyte transducer material. The $LaCr_xCo_{1-x}O_3$ layers were prepared with a polymeric precursor method that used ethylene glycol as the solvent, acetyl acetone as the chelating agent, and polyvinylpyrrolidone as the polymer additive. The effects of the Co concentration on the structural, morphological, and $NO_x$ sensing properties of the $LaCr_xCo_{1-x}O_3$ powders were investigated with powder X-ray diffraction, field emission scanning electron microscopy, and its response to 20~250 ppm of $NO_x$ at $400^{\circ}C$ (for 1 kHz and 0.5 V), respectively. When the as-prepared precursors were calcined at $700^{\circ}C$, only a single phase was detected, which corresponded to a perovskite-type structure. The XRD results showed that as the Co concentration of the $LaCr_xCo_{1-x}O_3$powders increased, the crystal structure was transformed from an orthorhombic phase to a rhombohedral phase. Moreover, the $LaCr_xCo_{1-x}O_3$ powders with $0{\leq}x<0.8$ had a rhombohedral symmetry. The size of the particles in the $LaCr_xCo_{1-x}O_3$powders increased from 0.1 to $0.5{\mu}m$ as the Co concentration increased. The sensing performance of the stack-structured $LaCr_xCo_{1-x}O_3/Li_{1.3}Al_{0.3}Ti_{1.7}(PO_4)_3$ sensors was found to divide the impedance component between the resistance and capacitance. The response of these sensors to NO gas was more sensitive than that to $NO_2$ gas. Compared to other impedancemetric sensors, the $LaCr_{0.8}Co_{0.2}O_3/Li_{1.3}Al_{0.3}Ti_{1.7}(PO_4)_3$ sensor exhibited good reversibility and reliable sensingresponse properties for $NO_x$ gases.

• Journal of the Korean Magnetics Society
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• v.17 no.2
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• pp.65-70
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• 2007

In this paper, we composed the $LiFePO_4$ for the reversible use as the replacement material of the Li ion batteries and confirmed the good quality of the structure of the samples with the sintering temperature $675^{\circ}C,\;750^{\circ}C,\;and\;800^{\circ}C$ for 30 hours at nitrogen atmosphere. We also investigated the size of the particles through SEM picture and the change of the sintering temperature and the $Fe^{+3}$ content after charging the materials with 1 V, 160 mA and 3 V, 40 mA for 3 hours by Mossbauer spectroscopy. Also we can observe the increase on the $Fe^{+3}$ content at the charge condition and the increase of the amount ratio of the $Fe^{+3}$ ion only in sintering temperature $675^{\circ}C$ according to the increase of the electric charge. We cannot observe the change of the $Fe^{+3}$ ion in sintering temperature $800^{\circ}C$ after charging.

• YAKHAK HOEJI
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• v.7 no.4
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• pp.98-99
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• 1963

Compound III and IV were formed from I and II with $NH_{2}(CH_{2})_{3}NH_{2}$ respectively. Reduction of I with $LiAlH_{4}$ bollowed by $PoCl_{3}$ treatment affored VIII. Compound VI which was asumed by IR-data were obtained by treatment of $NH_{2}NH_{2}$ upon I or V.

• Korean Journal of Materials Research
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• v.22 no.7
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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 $300^{\circ}C$.

• Journal of Powder Materials
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• v.30 no.5
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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.

• Journal of Sensor Science and Technology
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• v.14 no.4
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• pp.258-264
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• 2005

Li+-ion conducting ($Li_{3}PO_{4}$) thin films with thickness of $0.3{\mu}m$, $0.65{\mu}$, $1.2{\mu}$ were deposited on $Al_{2}O_{3}$ substrate at room temperature by thermal evaporation. They were sintered at $700^{\circ}C$ and $800^{\circ}C$ for 2 hours, respectively. Reference electrode and sensing electrode were printed on Au-electrode by silk printing method. The EMF and the ${\Delta}EMF$/dec were increased with increasing the electrolyte thickness and sintering temperature. The sample sintered at $800^{\circ}C$ was shown a good response and recovery characteristics more than those sintered at $700^{\circ}C$. The Nernst's slop of 75 mV per decade was obtained at operating temperature of $500^{\circ}C$.

• Proceedings of the Materials Research Society of Korea Conference
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• 2003.03a
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• pp.216-216
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• 2003

현재 상용화되어 있는 리튬 이차전지용 양극재료로는 비교적 작동전압이 높은 층상 암염구조(LiCoO$_2$, LiNiO$_2$) 및 Spinet계(LiMn$_2$O$_4$) 전이금속 산화물이 대부분 이용되고 있다 하지만 LiCoO$_2$나 LiNiO$_2$ 같은 상용화 물질은 비교적 높은 비용과, 강한 독성 때문에 많은 문제점을 가지고 있다. 또 Spinel(LiMn$_2$O$_4$)는 낮은 비용과 환경친화적인 장점에도 불구하고 Jahn-Teller 변형과 관련된 구조적 변형이 심각하기 때문에 사이클시 비가역적인 용량의 감소가 심각하다. 이러한 관점에서 전이금속보다 그 양이 풍부하고 저렴할 뿐만 아니라 독성이 없는 Olivine 구조 (LiFePO$_4$)를 갖는 phosphate계 화합물에 관심을 가지게 되었다. LiFePO$_4$는 리튬 음극과 3.4V의 방전전압을 나타내며, 170mAh/g의 이론용량을 가지고 있어, Fe-base의 장점은 물론 안정적인 결정구조 및 현재 상용화된 재료들과 비슷한 에너지 밀도를 가진다. 따라서 본 연구에서는 양극물질의 기존 두 제조법인 고상반응법과 sol-gel법으로 대표되는 제조법의 단점을 상호 보완될 수 있다고 판단되는 기계적 합금화법(Mechanical Alloying, MA)공정을 도입하여 초미세립 분말 제조에 초점을 맞추어 Olivine phosphate계 양극물질의 제조 및 전기화학적 특성을 연구하였다.

• Journal of Powder Materials
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• v.30 no.2
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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.

• Polymer(Korea)
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• v.25 no.1
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• pp.6-14
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• 2001

The monomer N,N'-bis(3-pyrrol-1-yl-propyl)-4,4'-bipyridinium$(PF_6)_2$ was electrochemically polymerized on glassy carbon electrode surface. This polymer film electrode has electroactive sites on its bipyridinium ions distributed at the polymer strands. The formal potentials of the electrodes were -0.41V and -0.81V(vs. SSCE) for each step at phosphate buffer(pH=5.70). The diffusion coefficients of the dopants ions into the polymer matrix were $1.57{\times}10^{-4}$ and $4.35{\times}10^{-5}cm^2s^{-1}$ for first and second redox couple, respectively. The rate constants of electron transfer at $V^{2+/+}$ of the first step was a $57.53s^{-1}$, which was 22 times higher than $V^{+/0}$ one having $2.63s^{-1}$ in the solution. The charge transfer resistance of the polymer film was influenced by the dopant ion of the electrolyte. Thus the resistances were 22.63, 16.81, 12.44 and $11.36k{\Omega}$ for $LiClO_4,\;NaClO_4,\;KClO_4$, and phosphate buffer, respectively. The reaction order of the electropolymerization was first order and the rate constant of the polymerization was $1.31{\times}10^{-1}s^{-1}$ as determined by EQCM method. The G.C./p-BPB type electrode doped with phosphate ions showed a stability and reproducibility in CV procedure over 20 cycles.