• 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.

• Journal of Powder Materials
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• v.30 no.4
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• pp.324-331
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• 2023

Lithium (Li) is a key resource driving the rapid growth of the electric vehicle industry globally, with demand and prices continually on the rise. To address the limited reserves of major lithium sources such as rock and brine, research is underway on seawater Li extraction using electrodialysis and Li-ion selective membranes. Lithium lanthanum titanate (LLTO), an oxide solid electrolyte for all-solid-state batteries, is a promising Li-ion selective membrane. An important factor in enhancing its performance is employing the powder synthesis process. In this study, the LLTO powder is prepared using two synthesis methods: sol-gel reaction (SGR) and solid-state reaction (SSR). Additionally, the powder size and uniformity are compared, which are indices related to membrane performance. X-ray diffraction and scanning electron microscopy are employed for determining characterization, with crystallite size analysis through the full width at half maximum parameter for the powders prepared using the two synthetic methods. The findings reveal that the powder SGR-synthesized powder exhibits smaller and more uniform characteristics (0.68 times smaller crystal size) than its SSR counterpart. This discovery lays the groundwork for optimizing the powder manufacturing process of LLTO membranes, making them more suitable for various applications, including manufacturing high-performance membranes or mass production of membranes.

• Journal of the Korean Electrochemical Society
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• v.3 no.2
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• pp.115-120
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• 2000

All solid-state thin film micro-batteries consisting of lithium metal anode, an amorphous LiPON electrolyte and cathode of vanadium oxide have been fabricated and characterized, which were fabricated with cell structure of $Li/LiPON/V_2O_5Pt$. The effect of various oxygen partial pressure on the electrochemical properties of vanadium oxide thin films formed by d.c. reactive sputtering deposition were investigated. The vanadium oxide thin film with deposition condition of $20\%\;O_2/Ar$ ratio showed good cycling behavior. In in-siか process, the LiPON electrolyte was deposited on the $V_2O_5$ films without breaking vacuum by r.f. magnetron sputtering at room temperature. After deposition of the amorphous LiPON, the Li metal films were grown by a thermal evaporator in a dry room. The charge-discharge cycle measurements as a function of current density and voltage variation revealed that the $Li/LiPON/V_2O_5$ thin film had excellent rechargeable properly when current density was $7{\mu}A/cm^2$. and cut-off voltage was between 3.6 and 2.7V In practical experiment, a stopwatch ran on this $Li/LiPON/V_2O_5$ thin film micro-battery. This result means that thin film micro-battery fabricated by in-siか process is a promising for power source for electronic devices.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.37 no.3
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• pp.274-279
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• 2024

Eu³⁺-doped BaZrO₃ (BaZrO₃:Eu³⁺) phosphor powders were prepared using a solid-state reaction by changing the molar concentration of Eu³⁺ within the range of 0.5 to 30 mol%. Irrespective of the molar concentration of Eu³⁺ ions, the crystal structures of all the phosphors were cubic. The excitation spectra of BaZrO₃:Eu³⁺ phosphors consisted of an intense broad band centered at 277 nm in the range of 230~320 nm. The emission spectra were composed of a dominant orange band at 595 nm arising from the ⁵D₀→⁷F₁ magnetic dipole transition of Eu³⁺ and two weak emission bands centered at 574 and 615 nm, respectively. As the concentration of Eu³⁺ increased from 0.5 to 10 mol%, the intensities of all the emission bands gradually increased, approached maxima at 10 mol% of Eu³⁺ ions, and then showed a decreasing tendency with further increase in the Eu³⁺ ions due to the concentration quenching. The critical distance between neighboring Eu³⁺ ions for concentration quenching was calculated to be 11.21 Å, indicating that dipole-dipole interaction was the main mechanism of concentration quenching of BaZrO₃:Eu³⁺ phosphors. The results suggest that the orange emission intensity can be modulated by doping the appropriate concentration of Eu³⁺ ions.

• Journal of Energy Engineering
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• v.20 no.2
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• pp.109-122
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• 2011

The production capacity of EV models should be sufficient to achieve the goal of one million EVs by 2015. Large-Format lithium-ion battery are expected to find a prominent role as ideal electrochemical storage systems in traction power train for sustainable vehicles such as all-electric vehicles. This review focuses first on the present status of production lithium-ion battery technology and cooperative relations of between battery and EV makers, then on its near future development.

• Journal of the Korean Electrochemical Society
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• v.11 no.2
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• pp.100-104
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• 2008

Titanium sheet metal substrates used in thin film batteries were wet etched and their surface area was increased in order to increase the discharge capacity and power density of the batteries. To obtain a homogeneous etching pattern, we used a conventional photolithographic process. Homogeneous hemisphere-shaped wells with a diameter of approximately $40\;{\mu}m$ were formed on the surface of the Ti substrate using a photo-etching process with a $20\;{\mu}m{\times}20\;{\mu}m$ square patterned photo mask. All-solid-state thin film cells composed of a Li/Lithium phosphorous oxynitride (Lipon)/$LiCoO_2$ system were fabricated onto the wet etched substrate using a physical vapor deposition method and their performances were compared with those of the cells on a bare substrate. It was found that the discharge capacity of the cells fabricated on wet etched Ti substrate increased by ca. 25% compared to that of the cell fabricated on bare one. High discharge rate was also able to be obtained through the reduction in the internal resistance. However, the cells fabricated on the wet etched substrate exhibited a higher degradation rate with charge-discharge cycling due to the nonuniform step coverage of the thin films, while the cells on the bare substrate demonstrated a good cycling performance.

• Journal of the Korean Electrochemical Society
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• v.3 no.1
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• pp.44-48
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• 2000

Amorphous $V_2O_5$ cathode thin films were prepared by DC-magnetron sputtering at room temperature and the thin film rechargeable lithium batteries were fabricated with the configuration of $V_2O_5/LIPON/Li$ using sequential ex-situ thin film deposition techniques. The electrochemical characteristics of $V_2O_5$ cathode materials Prepared at 80/20 of $Ar/O_2$ ratio showed high capacity and cycling behaviors by half cell test. LIPON solid electrolytes films were prepared by RF-magnetron sputtering using the self-made $Li_3PO_4$ target in pure $N_2$ atmosphere, and it was very stable for lithium contact in the range of 1.2-4.0 V vs. Li. Metallic lithium were deposited on LIPON electrolyte by thermal evaporation methode in dry room. Vanadium oxide based full cell system showed the initial discharge capacity of $150{\mu}A/cm^2{\mu}m$ in the range of $1.2\~3.5V$.

• 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 the Korean Electrochemical Society
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• v.3 no.4
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• pp.219-223
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• 2000

All-solid state lithium rechargeable thin film batteries were fabricated with the configuration of$Cu_{0.5}V_2O_5/Lipon/Li$ using sequential thin film techniques. Copper vanadium oxide thin films and Lipon thin films were prepared by DC reactive dual source magnetron sputtering and RF magnetron sputtering, respectively. According to XRD analysis, we found out that copper vanadium oxide thin films were amorphous. The electrochemical behaviour of them was examined in half cell system using EC : DMC(1:1 in IM $LiPF_5$) liquid electrolyte. The ionic conductivity of Lipon thin film was $1.02\times10^{-6}S/cm$ at $25^{\circ}C$ and $Cu_{0.5}V_2O_5/Lipon/Li$ cell showed that the discharge capacity was about $50{\mu}Ah/cm^2{\mu}m$ beyond 500cyc1es.

• Journal of the Korean Electrochemical Society
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• v.24 no.3
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• pp.52-64
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• 2021

The effect of Fe and BO₃ doping on structure, thermal, and electrical properties of Li_1+xFe_xTi_2-x(PO₄)_3-y(BO₃)_y (x = 0.2, 0.5)-based glass and glass ceramics was investigated. In addition, their crystallization behavior during sintering and ionic conductivity were also investigated in terms of sintering temperature. FT-IR and XPS results indicated that Fe²⁺ and Fe³⁺ ions in Li_1+xFe_xTi_2-x(PO₄)_3-y(BO₃)_y glass worked as a network modifier (FeO₆ octahedra) and also as a network former (FeO₄ tetrahedra). In the case of the glass with low substitution of BO₃, boron formed (PB)O₄ network structure, while boron preferred BO₃ triangles or B₃O₃ boroxol rings with increasing the BO₃ content owing to boic oxide anomaly, which can result in an increased non-bridging oxygen. The glass transition temperature (GTT) and crystallization temperature (CT) was lowered as the BO₃ substitution was increased, while Fe²⁺ lowered the GTT and raised the CT. The ionic conductivity of Li_1+xFe_xTi_2-x(PO₄)_3-y(BO₃)_y glass ceramics were 8.85×10^-4 and 1.38×10^-4S/cm for x = 0.2 and 0.5, respectively. The oxidation state of doped Fe and boric oxide anomaly were due to the enhanced lithium ion conductivity of glass ceramics.