• Proceedings of the KIEE Conference
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• 2005.07c
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• pp.1989-1991
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• 2005

Lithium titanium oxide as anode material for energy storage prepared by novel synthesis method. $Li_4Ti_5O_{12}$ based spinel-framework structures are of great interest material for lithium-ion batteries. We describe here $Li_4Ti_5O_{12}$ a zero-strain insertion material was prepared by novel sol-gel method and by high energy ball milling (HEBM) of precursor to from nanocrystalline phases. According to the X-ray diffraction and scanning electron microscopy analysis, uniformly distributed $Li_4Ti_5O_{12}$ particles with grain sizes of 100nm were synthesized. Lithium cells, consisting of $Li_4Ti_5O_{12}$ anode and lithium cathode showed the 173 mAh/g in the range of $1.0{\sim}3.0V$. Furthermore, the crystalline structure of $Li_4Ti_5O_{12}$ didn't transfer during the lithium intercalation and deintercalation process.

• Proceedings of the KAIS Fall Conference
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• 2003.06a
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• pp.181-184
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• 2003

ZnwO₄는 높은 품질계수에 의해 주파수 선택성이 뛰어나지만 다층형태의 고주파 무선부품으로의 응용을 위해서는 높은 소결온도(1100℃), 큰 음의 공진주파수 온도계수(-70ppm/℃), 낮은 유전율(15.5) 둥에 대한 보정이 필요하다. 본 연구에서는 ZnwO₄에 TiO₂ 및 LiF를 첨가하여 ZnwO₄의 저손실특성을 유지하면서 주파수 온도안정성 및 저온소결성을 부여하고자 하였다. 큰 양의 공진주파수 온도계수(＋400ppm/℃) 및 유전율(100)을 갖는 TiO₂의 첨가는 공진주파수 온도계수를 음의 값에서 양의 값으로 변화시켰으며 유전율의 증가를 가져왔다. TiO₂를 20 mol％ 첨가한 경우 공진주파수 온도 계수가 0에 가깜고 유전율 19.4에 품질계수 50000㎓의 특성을 얻을 수 있었으나 소결온도는 1100℃로 높은 소결온도를 보였다. ZnwO₄에 TiO₂가 첨가된 혼합체에 LiF의 첨가는 액상형성에 의해 소결온도를 1100℃에서 850℃로 크게 저하시킬 수 있었다. LiF는 첨가는 LiF 자체의 큰 공진주파수 온도계수에 의해 온도계수를 음의 값으로 변화시켰다. 따라서 TiO₂ 및 LiF의 적당량의 첨가는 온도 안정성을 갖는 저손실 ZnwO₄-TiO₂-LiF계 LTCC 소재를 제조할 수 있었다.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2008.06a
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• pp.55-55
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• 2008

이차전지의 음극 중 $LiC_6$는 높은 용량을 보이나 완충하는 프로세스 동안에 금속리튬에 가까운 potential을 갖게 되어 조작에 어려움이 있다. 이러한 대용물질로서 $Li_4Ti_5O_{12}$ spinel은 가볍고 높은 에너지 밀도를 가지고 있고 낮은 전압영역이 가능하여 이차전지의 음극 물질로서 유용하다. 그러나 $Li_4Ti_5O_{12}$ 물질 자체가 insulation이며, 고상합성법을 사용하게 되면 좋은 특성을 나타내기가 어렵다. 이번 실험에서는 고상합성을 통하여 $Ba^{2+}$와 $Sr^{2+}$이온을doping한 후 전기화학적 특성이 어떻게 향상되었는가를 연구하였다. Ba와 Sr을 첨가한 $Li_4Ti_5O_{12}$는 첨가하지 않은 물질에 비하여 보다 안정적인 평탄구역을 갖게 되었으며 방전용량이 $40mAhg^{-1}$의 향상을 가져왔다. 또한 Li half cell에서 100cycle 진행하는 동안 보다 안정적인 전극구조를 유지하였다.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2009.11a
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• pp.262-262
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• 2009

최근 리튬이차전지가 전지자동차, hybrid car, PHEV, Ev, UPS 저장장치로 사용되기 시작함에 따라 고용량화, 고출력화가 요구되고 있다. 현재까지 주로 사용 되어왔던 carbon으로는 작동전압이 낮고, 고용량화, 고출력화가 어려워 금속산화물, 금속 비정질 금속 및 금속산화물을 carbon과 혼합 사용 함으로써 차세대 전지로서 특성을 달성하고 있다. 따라서 본 연구에서는 음극 소재로서 안정성이 뛰어난 금속산화물로 $Li_4Ti_5O_{12}$를 합성할 때 저가의 $TiCl_4$를 이용 $Li_4Ti_5O_{12}$가 고밀도를 갖게끔 $TiCl_4$를 이용 구형의 Ti-precursor(전구체)를 합성한 후 구형의 $Li_4Ti_5O_{12}$를 합성하였다. Ti전구체는 $TiCl_4$로부터 합성하였는데 이때 구형을 제조하고자 Hydroxypropyl cellulose(이하 HPC)를 사용하여 반응을 진행하였다. 이때 반응 조건 및 HPC의 몰수 변화에 따른 입자 형상의 변화에 관하여 관찰한 결과, $TiOCl_2$ 0.4mol, 반응온도 $10^{\circ}C$, 유지시간 6시간, HPC양 0.02mol일 때 $0.6{\mu}m$ 정도의 구형 Ti-전구체를 합성하였다. 합성된 Ti-전구체와 리튬수화물을 사용하여 $Li_4Ti_5O_{12}$를 합성 하였고, 상기 물질로 전지특성을 평가하였다.

• Electrical & Electronic Materials
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• v.10 no.9
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• pp.901-908
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• 1997

The microwave dielectric properties of (Na.$_{1}$2//Sm$_{1}$2/)TiO$_3$and (Li$_{1}$2//Nd$_{1}$2/)TiO$_3$ceramics were investigated. Dielectric constant quality factor and temperature coefficient of resonant frequency of (Li$_{1}$2//Nd$_{1}$2/)TiO$_3$ceramics sintered at 145$0^{\circ}C$ for 2 hours were 86.2, 2780(at 3.8GHz) and 215ppm/$^{\circ}C$respectively. The solid solution of X(Na.$_{1}$2//Sm$_{1}$2/)TiO$_3$-(1-X)(Li$_{1}$2//Nd$_{1}$2/)TiO$_3$increased delectric constant and quality factor were decreased. Whereas temperature coefficient of resonant frequency was optimized to zero at the composition of 0.6(Li$_{1}$2//Sm$_{1}$2/)TiO$_3$-0.4(Li$_{1}$2//Nd$_{1}$2/)TiO$_3$where dielectric constant and quality factor were 86.2, 95-(at 3.8GHz) respectively. Also band-pass filters made of this material were examined.

• Proceedings of the KAIS Fall Conference
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• 2010.11a
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• pp.110-114
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• 2010

Li-incorporated mesoporous $TiO_2$ materials with various pore-sized istributions were synthesized by using triblockcopolymers via a sol-gel process in a queous solution. The properties of the se materials were characterized by HR-TEM, XRD, and BET analysis. All particles have spherical morphology with a diameterrange of $1-3{\mu}m$. The mesoporous $TiO_2$ materials calcined at $400^{\circ}C$ and their specific surface area, average pore size and crystallite sizes were 210 $m^2g^{-1}$, 6.4 nm and 8.8 nm respectively. The Li-incorporated mesoporous $TiO_2$ were tested for $CO_2$ adsorption and its adsorption capacity is 90mg/g. The Li-incorporated mesoporous $TiO_2$ ar eobserved to be thermally stable, recyclable and greens or bent for $CO_2$ capture. The effect of bimetallic $ZrLiTiO_2$ is also studied for $CO_2$ adsorption.

• Journal of the Korean Ceramic Society
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• v.47 no.6
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• pp.627-632
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• 2010

In this paper the effect of the structure, particle size, morphology of nanofibers and nanoparticles for the electrochemical characteristics of $Li_4Ti_5O_{12}$ was investigated. The $H_2Ti_2O_5{\cdot}H_2O$ synthesized in hydrothermal treatment from a NaOH treatment on $TiO_2$ by ion exchange processing with HCl solutions. After the $Li_4Ti_5O_{12}$ nanofibers synthesized in hydrothermal treatment of $H_2Ti_2O_5{\cdot}H_2O$ and $LiOH{\cdot}H_2O$. The hydrogen titanate precursor prepared by ion exchange processing with 0.1~0.3M HCl solutions and the final products calcined at $350^{\circ}C{\sim}400^{\circ}C$. The $Li_4Ti_5O_{12}$ nanofibers showed well reversibility during the insertion and extraction of Li, good cycle performance, high capacity and low electrochemical reaction resistance than nanoparticles. also c-rate exhibited a discharge capacity of 172 mAh/g at 0.2C and 115mAh/g at 5C, which is the 77%, 67% of that obtained in the process charged, discharged at 0.2C.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2003.07a
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• pp.131-134
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• 2003

[ $ZnWO_4$ ] shows excellent frequency selectivity due to its high quality factor($Q{\times}f$) at microwave frequencies. However, in order to use $ZnWO_4$ as multilayered wireless communication components, its other properties such as sintering temperature($1050^{\circ}C$), ${\tau}_f$ ($-70ppm/^{\circ}C$) and ${\varepsilon}_r(15.5)$ should be modified. In present study, $TiO_2$ and LiF were used to improve the microwave dielectric and sintering properties of $ZnWO_4$. $TiO_2$ additions to $ZnWO_4$ changed ${\tau}_f$ from negative to positive value, and also increased ${\varepsilon}_r$ due to its high ${\tau}_f$ ($+400ppm/^{\circ}C$) and ${\varepsilon}_r$(100). At 20 mol% $TiO_2$ addition, ${\tau}_f$ was controlled to near zero $ppm/^{\circ}C$ with ${\varepsilon}_r=19.4$ and $Q{\times}f=50000GHz$. However, the sintering temperature was still high to $1100^{\circ}C$. LiF addition to the $ZnWO_4+TiO_2$ mixture was greatly reduced the sintering temperature from $1100^{\circ}C$ to $850^{\circ}C$ due to liquid phase formation. Also LiF addition decreased the ${\tau}_f$ value due to its high negative ${\tau}_f$ value. Therefore, by controlling the $TiO_2$ and LiF amount, temperature stable LTCC material in the $ZnWO_4$-TiO_2-LiF$ system could be fabricated.

• Journal of the Korean Ceramic Society
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• v.40 no.2
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• pp.178-183
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• 2003

Electrical conductivity of$50Li_2O-xTiO_2-(50-x)P_2O_5$ glasses has been studied with an increase of the intermediate$TiO_2$content. Thermal properties were observed from TG-DTA measurement and the variation of glass structure was investigated by FT-IR. The density and glass transition temperature increased with an increase of the $TiO_2$ content. These results were attributed to the fact that bond strengthening was occurred because of the formation of P-O-Ti cross linkages in the glass. The ionic conductivity increased with $TiO_2$ content and a maximum value, $1.2{imes}10^{-6}$S/cm showed at x=20. The ionic conductivity showed a large increasement as a result that the pyrophosphate group become the predominant structural unit. This result can explain that Li ions mobility increased as a number of non-bridging oxygen on phosphate units increased.

• Korean Journal of Materials Research
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• v.34 no.4
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• pp.185-193
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• 2024

In this study, NASICON-type Li_1+XGa_XTi_2-X(PO₄)₃ (x = 0.1, 0.3 and 0.4) solid-state electrolytes for all-solid-state batteries were synthesized through the sol-gel method. In addition, the influence on the ion conductivity of solid-state electrolytes when partially substituted for Ti⁴⁺ (0.61Å) site to Ga³⁺ (0.62Å) of trivalent cations was investigated. The obtained precursor was heat treated at 450 ℃, and a single crystalline phase of Li_1+XGa_XTi_2-X(PO₄)₃ systems was obtained at a calcination temperature above 650 ℃. Additionally, the calcinated powders were pelletized and sintered at temperatures from 800 ℃ to 1,000 ℃ at 100 ℃ intervals. The synthesized powder and sintered bodies of Li_1+XGa_XTi_2-X(PO₄)₃ were characterized using TG-DTA, XRD, XPS and FE-SEM. The ionic conduction properties as solid-state electrolytes were investigated by AC impedance. As a result, Li_1+XGa_XTi_2-X(PO₄)₃ was successfully produced in all cases. However, a GaPO₄ impurity was formed due to the high sintering temperatures and high Ga content. The crystallinity of Li_1+XGa_XTi_2-X(PO₄)₃ increased with the sintering temperature as evidenced by FE-SEM observations, which demonstrated that the edges of the larger cube-shaped grains become sharper with increases in the sintering temperature. In samples with high sintering temperatures at 1,000 ℃ and high Ga content above 0.3, coarsening of grains occurred. This resulted in the formation of many grain boundaries, leading to low sinterability. These two factors, the impurity and grain boundary, have an enormous impact on the properties of Li_1+XGa_XTi_2-X(PO₄)₃. The Li_1.3Ga_0.3Ti_1.7(PO₄)₃ pellet sintered at 900 ℃ was denser than those sintered at other conditions, showing the highest total ion conductivity of 7.66 × 10^-5 S/cm at room temperature. The total activation energy of Li-ion transport for the Li_1.3Ga_0.3Ti_1.7(PO₄)₃ solid-state electrolyte was estimated to be as low as 0.36 eV. Although the Li_1+XGa_XTi_2-X(PO₄)₃ sintered at 1,000 ℃ had a relatively high apparent density, it had less total ionic conductivity due to an increase in the grain-boundary resistance with coarse grains.