• Journal of the Korean Ceramic Society
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• v.37 no.12
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• pp.1178-1186
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• 2000

타일의 내마모성과 내산성을 향상시키기 위해 결정화유리가 최근에 새로운 유약 재료로서 소개되고 있다. 신 유약의 연구에 사용된 조성은 $Ca_2$ZrSi$_4$O$_{12}$ 상에 근접하는 CaO-ZrO$_2$-SiO$_2$계의 유리조성의 분말로, 마이크로파 가열 (2.45 GHz)에 의해서 900-120$0^{\circ}C$의 0-20분간 소성되어 평가되었다. 그 결과, 100$0^{\circ}C$ 이상에서 소성한 시편은 내부 결정화를 나타내었으며, 결정상은 미세(5$mu extrm{m}$)한 크기를 갖는 $Ca_2$ZrSi$_4$O$_{12}$가 주 결정상이며, $Ca_2$ZrSi$_4$O$_{12}$, CaSiO$_3$, SiO$_2$의 세 상이 나타났다. 소결체의 미세구조는 사용한 유리분말의 입도의 영향을 받았다. 미세분말 (<38$\mu\textrm{m}$)을 이용한 소결체의 조직이 조세분말 (45-150$\mu\textrm{m}$)의 경우보다 수축율면에서 높았으며 낮은 기공도를 갖는 미세구조를 가졌다. 마이크로파에 의한 유리분말의 소성은 1000-120$0^{\circ}C$ 구간에서 10분 이내 결정화가 완료되는 급속 가열 공정이었으며 CaO-ZrO$_2$-SiO$_2$계 결정화 유리 제조에 균일한 체적가열을 할 수 있었다.

• Proceedings of the Materials Research Society of Korea Conference
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• 2003.11a
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• pp.98-98
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• 2003

초내열성 결정화유리는 전기전자부품, 천체만원경의 반사경, 직화용 조리기기, 군사용 부품 등에 광범위하게 이용되고 있는데 이중 LAS 계가 가장 오랫동안 알려진 조성 계이다. 이 결정화유리는 주입성형후 열처리에 의하여 결정상을 생성하여 사용되는데 표면이 매우 낮은 조도를 갖는 것으로 알려져 있으나 실제로는 제조상에 조도가 높게 나타나는 문제점이 제기되고 있다. 따라서 본 연구에서는 미세조직적인 측면에서 이러한 점을 연구하고자 Li$_2$O-AL$_2$O$_3$-SiO$_2$를 주성분으로 하고 소량의 MgO와 핵생성제로서 TiO$_2$, ZrO$_2$를 사용하여 시편을 제조하였다. 제조된 결정화유리의 결정화도의 차이에 따라 AFM, $\alpha$-STEP등으로 표면의 조도를 정량화였다. 결정상의 종류, 크기, 결정화도, 결정상간의 간격 등이 표면의 조도에 어떻게 영향을 주는가 에 대하여 연구한 결과를 제시하였다.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.17 no.2
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• pp.82-89
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• 2007

Glass-ceramics were fabricated by heat-treating a glass at $700^{\circ}C$/10hr which was obtained by melting a glass frit mixed with $40{\sim}80 wt%$ EAF dust at $1300^{\circ}C$/1hr. Dependence of crystal phase and bonding state change upon a compositional change and heat treatment condition were studied and the results was connected to the toxic characterization leaching procedure (TCLP) test data to investigate a chemical durability of the specimens. Increasing dust in a glass shifted the peak around $1000cm^{-1}$ to the lower frequency which was composed of two vibration peaks for the nonbridging oxygen at $960cm^{-1}$ and the bridging oxygen at $1050{\sim}1060cm^{-1}$. Also, the $B_2O_3$ structure of boroxol ring changed to a tetrhedral-, trigonal- and di-borate with dust addition. The Fe-O peaks in the glass-ceramics were observed which is consitent with XRD results of spinel formation. The surface of glass after TCLP test was severely cracked while there was no cracks on a glass-ceramics after TCLP test so the chemical durability of the glass-ceramics is superior than that of glass. The leaching concentration of Fe for the glass-ceramics containing EAF dust 80 wt% is 1/15 times lower than that of glass. The Zn leaching concentration fur the glass-ceramics containing dust < 70 wt% was higher than that of glass but its trend was reversed for the specimen of dust content > 80 wt% which could be concluded as correlated with occurrence of willemite phase.

• Journal of the Korean Ceramic Society
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• v.39 no.6
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• pp.558-565
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• 2002

Coal fly ash, produced from a power plant in Korea was used for the production of glass-ceramics and the physical properties of glass-ceramics were evaluated. CaO and TiO$_2$ were added into the fly ash during the melting process to reduce the viscosity of molten glass and to induce internal crystallization of glass, respectively. Glass-ceramic was produced through a single stage heat treatment (at 950∼1050$\^{C}$ for 37∼240 min) after preparing glass (iota fly ash powder. As a result, a new tiny rod type crystals (a=7.4480, b=10.7381, c=4.3940 A, $\alpha$=94.9, $\beta$=98.6, γ=108.5°) was found in the glass-ceramics, which showed attractive mechanical properties, high hardness (7.1∼7.6 GPa) and wear resistance (by erosion test). Thus a glass-ceramic produced from thermal power plant fly ash and cell as a source for CaO exhibits a suitable treatment for the recycling and exploitation of waste materials and would be acceptable for a new application far building materials.

• Journal of the Korean Ceramic Society
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• v.38 no.12
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• pp.1137-1143
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• 2001

In this study, glass-ceramics containing cordierite(2MgO$.$2Al$_2$O$_3$5SiO$_2$) as a major crystalline phase was prepared from MAS (MgO-Al$_2$O$_3$-SiO$_2$) glass system for the application to reflector. Glasses prepared with addition of TiO$_2$as a nucleating agent were crystallized by two-step heat treatment of nucleation and crystal growth. Then nucleation and crystal growth behavior were investigated and the influence of heat treatment schedule on the nature of crystal phases and the diffuse reflectance spectrum was investigated. As a result, cordierite and rutile were precipitated as a major crystalline phases for the glass-ceramics with the nucleation at 750$^{\circ}C$ for 3 hours and then crystallization at 1100$^{\circ}C$ for 5 hours, and this glass-ceramics showed the reflectance over 90% in 570∼2500nm specturm region.

• Analytical Science and Technology
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• v.26 no.3
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• pp.205-210
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• 2013

For the synthesis of crystalline LAS glass by sol-gel method, the effect of operation conditions including metal alkoxide ratio, nucleating agent composition and heat treatment on the crystalline properties was experimentally investigated. The gelation time and crystallization temperature were proportionally affected by the mole ratio of TEOS in metal alkoxides solution. The addition of $TiO_2$ had an influence on the increasing of the gelation time, but the crystallization temperature was rarely dependent on the adding of nucleating agent. The crystallinity of LAS glass was improved by the nucleating agent under same heat treatment conditions.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.33 no.5
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• pp.181-186
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• 2023

In this study, novel Eu₂O₃-BaF₂-La₂O₃-B₂O₃ oxyfluoride glasses and glass ceramics were developed by a containerless processing. Differential thermal analysis (DTA) analysis was performed to analyze the thermophysical properties of oxyfluoride glasses doped with Eu₂O₃, and photoluminescence (PL) characteristics were analyzed to evaluate the luminous efficiency depending on the degree of crystallinity. The glass transition temperature decreased with increasing BaF₂ concentration since BaF₂ acts as a network modifier in this glass system. In addition, thermal stability which can be estimated by the difference between the glass transition temperature and the onset temperature of the crystallization decreased with increasing BaF₂ contents. The peak related to the BaF₂ crystal was confirmed after the crystallization by X-ray Diffraction (XRD) analysis. Photoluminescence intensity increased after the crystallization which indicates that the Eu³⁺ ions are sited in BaF₂ crystal. La 3d_5/2 x-ray photoelectron spectroscopy (XPS) and F1s XPS spectra were analyzed to precisely understand the behavior of the fluorine ion in the glass structure. Fluorine tends to bond with the network modifying cations such as La³⁺ and Ba²⁺ ions and after the crystallization the La-F bonds decreased because F^- ions used to form BaF₂ crystals.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.31 no.2
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• pp.84-88
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• 2021

The change of the photoluminescence properties of La2O3-CaF2-Al2O3-SiO2 glass-ceramics doped with rare earth material, that is used as laser and optical sensors, was analyzed according to heat treatment temperature. The heat treatment conditions for fabricating glass-ceramics were obtained through non-isothermal thermal analysis, and X-ray diffraction analysis was performed to determine the degree of crystal growth and kinds of crystal phases generated according to the heat treatment temperature. Using Scherrer's equation, it was predicted that crystals with a size of 25~40 nm would be generated inside the glass-ceramics. Photoluminescence (PL) analysis showed that the specimens heat-treated at 660℃ to 670℃ for 1 hour had the highest PL intensity. Also, from the CIE color coordinate analysis, all glass-ceramics specimens emitted red-orange light regardless of the heat treatment condition.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.1 no.2
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• pp.94-103
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• 1991

ZnO-$P_2O_5$ system glasses containing 45 to 60 mol% ZnO have been melted at$1200^{\circ}C$and crystallized through controlled heat treatment. The properties of the base glass and crystallized glass were examined with XRD. FTIR. density. thermal expansion, electric conductivity, hardness. The principal crystalline phase was identified as zinc metaphosphate [$Zn(PO_3)_2$ in crystallized glasses containing 45-55mol% ZnO and zinc pyrophosphate ($Zn_2P_2O_7$) in the sample of 60mol% ZnO with X - ray diffraction analysis. Thermal expansion coefficient and DC electrical conductivity were varied with direction of oriented crystalline in the samples containing 50-60mol% ZnO. This suggests the existance of the oriented crystalline.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.10 no.6
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• pp.407-411
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• 2000

Low-temperature solder glass for use in electronic package was experimentally prepared and its crystallization behavior was investigated using differential thermal analysis (DTA) under nonisothermal condition. The composition of the solder glass was determined from PbO-ZnO-$B_2$$O_3$-$TiO_2$ glasses containing small amounts of CaO, $SiO_2$$A1_2$$O_3$ and $P_2$$O_5$. The crystallization exotherm corresponding to the formation of lead titanate (PbTiO$_3$) was observed. The crystallization of $PbTiO_3$was a three-dimensional process with the average activation energy of 223$\pm$3 kJ/mol for the crystallization from the glass matrix.