• Journal of the Korean Ceramic Society
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• v.32 no.2
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• pp.171-182
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• 1995

Five eucryptite and ten spodumene compositional powders were syntehsized from three sillimanite group, two kaolin group, and five pyrophyllite group silicate minerals. Those powders were isotatically pressed and fired at 1200~135$0^{\circ}C$ for 2 hrs, and then the sintered bodies were characterized. Silicate minerals with molar ratio of Al2O3 to SiO2 correspond to those of eucryptite and spodumene are kaolin and pyrophyllite group silicate minerals, respectively. Sintering characteristics of eucryptite from kaolin group and spodumene from pyrophyllite group mineral were superior to those from other silicate minerals. Eucryptite sintered bodies with 95~97% relative densities and densified microstructures can be obtained using Hadong pink kaolin as starting materials by sintering over broad temperature zone(1250~135$0^{\circ}C$). The eucryptite sintered bodies which were fired at 130$0^{\circ}C$ for 2hrs, from Hadong pink kaolin had within 3.0wt% microstructural compositional variations compaired with stoichiometric compound, and had good negative thermal expansiion property with -3.55$\times$10-6/$^{\circ}C$ thermal expansion coefficient. Spodumene sintered bodies which were prepared from pyrophyllite group silicate minerals, had dense microstructures and high densities by densification through liquid phase sintering with enlarged temperature range. The specimens which were fired at 130$0^{\circ}C$ for 2 hrs from Gusipyrophillite, had dense microstructure with crystallines mainly, and low thermal expansion property with 0.62$\times$10-6/$^{\circ}C$ thermal expansion coefficient. The porous texture and residual glass phase in LAS system ceramics which were prepared from silicate minerals, tend to increase the thermal expansion properties of sintered bodies to positive direction.

• Journal of the Korean Ceramic Society
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• v.31 no.5
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• pp.572-580
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• 1994

With low thermal expansion coefficients, eucryptite (Li2O.Al2O3.2SiO2) and spodumene (Li2O.Al2O3.4SiO2) in LAS ceramic system show good thermal shock resistance. In this study, sillimanite or kaolin group silicate minerals and Li2CO3 were used as starting materials, and if necessary SiO2 or Al2O3 were added for making stoichiometrically formed specimens. By this process, eucryptite powders were synthesized and characterized. The powder mixtures of lithiumcabonate and silicate minerals calcined at 80$0^{\circ}C$ for 2 hrs were made into powder compacts. $\beta$-Eucryptite single phase was formed via intermediate phases of Li2SiO3 and LiAlO2 et al, by heating at 110$0^{\circ}C$ or 120$0^{\circ}C$ for 10 hrs from those powder compacts. When using the sillimanite group minerals, Virginia kyanite or andalusite was reacted to form eucryptite at 120$0^{\circ}C$and CMK International kyanite were completed at 110$0^{\circ}C$. When kaolin group minerals were used, it was found that the synthesizing temperature (100$0^{\circ}C$) of $\beta$-eucryptite from the mixture of New Zealand white kaolin was lower than that from Hadong pink kaolin (110$0^{\circ}C$). The Microstructure of systhesized powder showed the irregular lump shape such as densed crystallines.

• Progress in Medical Physics
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• v.3 no.1
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• pp.9-18
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• 1992

In this study, beta-eucryptite is fabricated and the thermal parameters of this material have been investigated. The thermoluminescence from 4MeV X-ray irradiated beta-eucryptite have been measured over the temperature range of 300K-600K. Thermoluminescence curve from X-ray irradiated beta-eucryptite shows five peaks located at 342K, 392K, 438K, 474K, and 527K. $\tau$, $\delta$ and $\omega$ of peak at 527K are 35K, 39K and 74K, respectively and this peak is found to be 2nd order kinetics. The activation energy of peak shape method is calculated to be 1.03eV and the frequency factor for 527K curve is calculated to be 3.9x10$\^$8/sec$\^$-1/. Based on the various heating rates methods, the activation energy of the peak is computed to be 1.02${\pm}$0.05eV that is similar to 1.19${\pm}$0.03eV of initial rise method. The linearity of thermoluminescence intensity and radiation flux is valid up to 50Gy and beyond higher dose the supralinearity and saturation come out.

• Journal of the Korean Ceramic Society
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• v.28 no.5
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• pp.415-421
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• 1991

Influence of Li2O.4B2O3 frit addition on the microstructure and thermal expansion properties of $\beta$-eucryptite ceramics was studied. With 1.0~10.0wt% frit addition, sintering temperature range was enlarged and densified body was obtained. Thermal expansion was increased from -6.67$\times$10-6 $^{\circ}C$-1 of pure sintered body to 1.03$\times$10-6$^{\circ}C$-1 of 6 wt% added body, but this increasement was accompanied by inhibition of thermal expansion anisotropy, so that improved microcracking property.

• Progress in Medical Physics
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• v.3 no.2
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• pp.23-31
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• 1992

The thermally stimulated luminecence (Thermoluminescence:TL) of manufactured beta-eucryptite was studied for dose range of 200cGy-20000Gy. The TL spectrum from cesium irradiated beta-eucryptite was measured over the temperature range of 300K to 600K. The linearity of TL intensity vs irradiation dose is valid up to 50Gy and beyond higher dose supralinearity and saturation come out. At the dose of 2000Gy, the net number of supralinearity is maximum. The net amount of supralinearity form newly formed trapping center by photon irradiation and totally calculated TL intensity are accord with the experimental results except for the 50Gy range that supralinearity appears.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2009.11a
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• pp.181-181
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• 2009

전자부품용 Pb-free sealing frit의 열팽창계수를 기판에 matching 시키기 위하여 음의 열팽창계수를 가지고 있는 $\beta$-Eucryptite, $\beta$-Spodumene를 합성하여 filler로 첨가하였다. 합성된 filler는 저온소성용 유리프리트의 높은 열팽창계수를 조절하기 용이하고, 유리프리트와 복합화 하여 소성하면 낮은 열팽창계수로 인한 우수한 열충격 저항성을 갖는다. Filler로써 $\beta$-Eucryptite, $\beta$-Spodumene의 결정성을 향상시키기 위해 $1250^{\circ}C$에서 5 시간 동안 유지하는 합성공정을 3회 반복 진행한 후 XRD를 사용하여 결정성을 분석하였고, TMA를 이용하여 filler 첨가량에 따른 유리프리트의 열팽장계수의 변화를 측정하였다. 또한, filler 입도와 함량에 따른 melting 특성을 분석하기 위해 Pill test를 진행하였으며, soda-lime glass 기판과의 접합면을 SEM을 사용하여 관찰하였다.

• Journal of the Korean Ceramic Society
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• v.22 no.3
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• pp.53-59
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• 1985

Nucleation and crystallization of $\beta$-eucryptite in a glass of molecular percentage composition Li2O.Al2O3.2SiO2 are studied. The glasses are made by quenching of the melts from 143$0^{\circ}C$ to room temperature. Heat-treatment for nucleation and crystal growth are caried out at various temperature in the range between 50$0^{\circ}C$ and 80$0^{\circ}C$ with different duration of time. The amounts of crystallization are estimated by the method of x-ray powder diffraction. As the results a time-temperature-transformation relation for crystallization is derived. The maximum rate of crystallization is observed at about 75$0^{\circ}C$ from the T-T-T-curve while the crystallization temperature is detected at 67$0^{\circ}C$ by DTA measurement. The crystallization temperature moved to 62$0^{\circ}C$ by adding 5 weight percents of TiO2 and it moved to 78$0^{\circ}C$ by adding 2 weight percents of V2O5. The crystallization temperature moved to 62$0^{\circ}C$ by adding 5 weight percent of TiO2 it moved to 78$0^{\circ}C$ by adding 2 weight percents of V2O5 The activation energy for crystallization from the pure glass is calculated as 68 Kcal/mol and it varied to 53 Kcal/mol and 110Kcal/mol when 5 weight percents of TiO2 and weight percents of V2O5 are added respectively.

• Journal of the Korean Ceramic Society
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• v.30 no.5
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• pp.381-388
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• 1993

Due to the anisotropy of thermal expansion, LAS system which has low thermal expansion property is hard to obtain a dense sintered body. Therefore, the thermal expansion coefficient and the mechanical strength were decreased. In this study, mullite, which has good mechanical properties in high temperature and comparatively low thmeral expansion coefficient, was taken as a additive in LAS system. And then, sintering, thermal, and mechanical properties were investigated. The results are follows; When mullite is added in eucryptite composition (Li2O.Al2O3.2SiO2) of LAS system, the creation of liquid phase results in the densification of sintered body and the specimen sintered at 136$0^{\circ}C$ for 2 hours shows optimum sintering condition. With the addition of mullite in eucryptite composition, mechanical strength is increased by the control of grain growth. Especially, flexual strength of EM0 specimen was about double value than the basic composition. Thermal expansion coefficients of EM0 and EM15 specimens sintered at 136$0^{\circ}C$ were -8.23$\times$10-6/$^{\circ}C$ and -4.90$\times$10-6/$^{\circ}C$ in the temperature range of RT.~80$0^{\circ}C$. As the mullite content are increased, negative thermal expansion ratios are decreased.

• Journal of the Korean Ceramic Society
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• v.32 no.1
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• pp.45-50
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• 1995

In order to densify LAS(Lithuim Aluminosilicate)system compounds, we used metal alkoxides as precursors. Also Mg was added by sol-gel method using metal alkoxides to the LAS system for improving the sinterability, thermal and mechanical properties. The result was that the synthesizing temperature was lowered about 10$0^{\circ}C$, the sintering temperature was lowered by over 10$0^{\circ}C$ and MOR of samples from metal alkoxides was two times larger than that of sample form oxide.

• Journal of the Korean Ceramic Society
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• v.32 no.11
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• pp.1233-1240
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• 1995

LAS system, which is difficult to be sintered, was densified by using the powder synthesized from metal alkoxides. Sinterability, thermal and mechanical properties were improved through synthesizing the complex oxide powder from the addition of Ge as an alkoxide. As a result, the synthesizing and sintering temperature of the LAS system lowered by about 10$0^{\circ}C$ and its modulus of rupture (MOR) increased twice higher compared to the sample from the oxide by the direct method.