• Journal of the Korean Ceramic Society
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• v.18 no.3
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• pp.187-191
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• 1981

The effect of additions, $TiO_2$ and $ZrO_2$ as nucleant on the base glass which composition was determined to 0.97 $Li_2O-Al_2O_3-SiO_2$ has been investigated by means of D.T.A., X-ray diffraction and dilatation. $TiO_2$ and $ZrO_2$ as nucleant were added 0.06mole, in which ratios of $TiO_2$/$ZrO_2$ were varied 1/0, 2/1, 1/1, 1/2 and 0/1. The crystalline phases were appeared to $\beta$-spodumene as principal, $\beta$-eucryptite and $ZrO_2$ as secondary, regardless of nucleant variations. The crystallinity of the crystallized glass added $TiO_2$, $ZrO_2$ mixture as nucleant was higher than that of the glass added $TiO_2$ or $ZrO_2$ only. The crystallinity of the glass added $TiO_2$/$ZrO_2$ =1/1 was highest. Increasing the addition of $ZrO_2$, it has been observed that the crystal growing temperature became higher.

• Journal of the Korean Ceramic Society
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• v.25 no.5
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• pp.541-551
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• 1988

The purpose of this investigation was to prepare multicomponent monolithic Li-Al-Si gels of composition(mol%) 16.67 Li2O-16.67 Al2O3-66.67 SiO2 and to convert the gels to monolithic glass-ceramic at low temperature without melting. The hydrolysis, DTA, TGA, TMA, SEM, pore distribution, density and the activation energy for crystallization of the glass-ceramic formation with rawmaterials of which tetraethl orhosilicate of networkforming cation(Si) is partially hydrolyzed, aluminum isoproxide and lithium methoxide prepared by Li-metal react with methanol were studied. The results were as follows : 1) Monolithic gels which were added with additional water, resulting in a total water content 2.5 to 3.0 times the stoichiometric amount required to fully hydrolyze the alkoxides. 2) Specimens were dried to form crylinders 60mm in length and 40mm in diameter in about 800 hrs at 5$0^{\circ}C$. 3) $\beta$-eucryptite crystals and $\beta$-spodumene crystals were detected in samples heated above 75$0^{\circ}C$. 4) Within the temperature and range of 25-50$0^{\circ}C$ and 1,00$0^{\circ}C$ the thermal expansion coefficient for crystallized samples were shown as 2.6-5.7$\times$10-7/$^{\circ}C$ and 7.4-12.5$\times$10-7/$^{\circ}C$, respectively. 5) The activation energy for the crystal growth was 11.01kcal/mol at 794$^{\circ}C$ to 85$0^{\circ}C$.

• Journal of the Korean Ceramic Society
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• v.48 no.4
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• pp.269-277
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• 2011

Glass-ceramics based on lithium disilicate($Li_2Si_2O_5$) are prepared by heat-treatment of glasses in a system of $SiO_2-Li_2O-K_2O-Al_2O_3$ with different compositions. The crystallization heat-treatment was conducted at the temperature range of $700{\sim}900^{\circ}C$ and samples were analyzed by XRD and SEM. Mechanical properties were determined by a Vicker's hardness and 4 point bending strength. When $SiO_2/Li_2O$ ratio increased, cristobalite and tridymite crystals showed more predominate than lithium disilicate crystals. Increase in $Al_2O_3$ contents in the glass suppressed crystallzation of lithium disilicate crystals. Increase in ZnO, $B_2O_3$ contents in the glass decreased crystallization temperature of lithium disilicate crystals, and increased mechanical properties because of the reduction of the lithium disilicate crystal size.

• Journal of the Korean Ceramic Society
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• v.44 no.8
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• pp.451-456
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• 2007

This paper presents results and observations obtained from a study of sintering behavior and crystallization in $Li_2O-Al_2O_3-SiO_2$ (LAS) Glass by screen printing method. The variable experimental conditions were determined carefully by Thermal-Mechanical Analyzer (TMA), Differential Thermal Analyzer (DTA) for setting the optimum transparent sintering conditions in LAS glass system, $10.5Li_2O-14.7Al_2O_3-58.1SiO_2-16.7B_2O_3(wt%)$, such as glass-ceramics which usually have low crystallization temperatures. Crystallization glasses generated during sintering was observed from diffraction patterns by X-Ray Diffraction (XRD), transmittance by UV-Vis spectrometer. Finally, the optimum sintering condition of LAS glass and the relation between factors and results in several sintering conditions were given by using Response Surface Methodology (RSM). From this study, we confirmed that crystallization interrupted densification during glass powder sintering. Furthermore, we observed that main effect of factors in glass powder sintering with concurrent crystallization depended on experimental conditions from main effects plot by MINTAB-14.

• 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.27 no.2
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• pp.288-296
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• 1990

Parent glasses for the experiments were prepared to be ratio of Li2O : Al2O3 : SiO2=4.5 : 25 : 70.5 as basic components, and TiO2 and ZrO2 in the mixing ratio of 1 : 1 were added as the nucleating agents, whose contents were increased in each sample. DTA, XRD, SEM, IR were observed, and thermal expansion and transmissivities were measured for the crystallized samples under the controlled heat-treatments. The transformation temperatures and the dilatometric softening temperatures in thermal expansion curves, and also the exothermic peaks in differential thermo-analytical curves were shifted to lower temperature. The crystal phase deposited through the heat-treatment was identified as ${\beta}$-quartz solid solution with XRD and IR analysis. The crystalline phases in oopactified samples were ${\beta}$-spodumene coexiting with ${\beta}$-quartz solid solution. The samples having more than 3% nucleating agents were transparent. The crystallized grain sizes were ranged 0.05 to 0.1$\mu\textrm{m}$. The crystallized transparent samples were exceeded 85% in the transmissivity.

• Proceedings of the KIEE Conference
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• 2002.07c
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• pp.1494-1496
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• 2002

내열 충격성 및 적외선 투과를 갖는 LAS($Li_2O-Al_2O_3-SiO_2$)계 글라스세라믹스를 제조하였다. 본 연구에서는 LAS계에 $TiO_2$를 핵형성제로, 점도를 감소시키기 위해 $P_2O_5$를 첨가하여 유리를 제조한 후, 글라스세라믹 결정상을 석출시켰다. 석출된 주 결정상은 ${\beta}$-eucryptite(SS)이었으며, 열팽창 계수가 거의 제로에 가까운 값을 얻었다. 또한 선택적인 스펙트럼의 흡수를 위한 color dopants에 대한 기초 자료 등이 조사되었다.

• Resources Recycling
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• v.31 no.4
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• pp.49-55
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• 2022

In this study, the heavy metal ions (of Pb, Cd, Cr, and Hg) in wastewater were removed using a spent Li₂O-Al₂O₃-SiO₂-based crystallized glass previously used as an induction top plate material. Changes in the removal efficiency of heavy metals according to different reaction parameters, such as the amount of zeolite used as a heavy-metal adsorbent, adsorption time, initial concentration of the heavy metals, and pH of the initial solution, were investigated. As the amount of zeolite added increased, the heavy-metal removal efficiency also increased. Adsorption time had a considerable influence on adsorption characteristics, and the removal efficiency of all heavy metals increased with increasing adsorption time. In the case of Cd, the removal efficiency was greatly improved depending on the adsorption time. The initial concentration of the heavy-metal solution did not affect the removal efficiency; however, the initial pH of the heavy-metal solution affected the removal efficiency. More specifically, the removal efficiency of Cd increased while that of Pb and Cr decreased with increasing pH. The adsorption characteristics of Hg were not significantly affected by pH.

• Journal of the Korean Ceramic Society
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• v.14 no.4
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• pp.230-235
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• 1977

In this paper the conditions of surface crystallization of glass were studied. The basic glass which is apt to crystallize, with $SiO_2$ 72.50, $Al_2O_3$ 5, 00, $Na_2O$ 8.00 $K_2O$ 3.50, CaO 5.00, MgO 3.00, $B_2O_3$ 3.00 Wt% is chosen. The strain point and softening point of this glass is 4$25^{\circ}C$ and 778$^{\circ}C$ each, and between the two temperatures we could get grystal on its surface by immersion in salt baths during some controlled hours. The kind of crystal on the surface of glass was confirmed by X-ray diffraction analysis and the change of the thickness of crystalline layers depending on temperature and time, was surveyed by using optical microscope. The results are as follows; 1. The chloride group is more suitable than sulfate group for the treating salt. 2. In the condition with 50 LiCl.50NaCl at 62$0^{\circ}C$ for 2 hrs and with 50 LiCL.20-30 NaCl.30-20 $CaCl_2$ at 72$0^{\circ}C$ for 15-20 min. we could get the best crystalline layers. 3. The crystal was silica-O and petalite with a little tridymite and nepheline. 4. The thickness of crystalline layers increased with increasement of temperature and time.

• Journal of the Korean Ceramic Society
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• v.26 no.6
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• pp.771-782
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• 1989

Synthesis of $\beta$-Sialon powder was attempted with carbothermal reduction of porous glass. The porous glass was prepared by heat and hydrothermal treatments of 9.32 Li2O.46.5B2O3.37.2SiO2.6.98Al2O3 glass. Carbon pyrolyzed from propane gas was deposited on the porous glass, thereafter activated carbon was added as reducing agents. The synthesized $\beta$-Sialon powder was pressureless sintered at 175$0^{\circ}C$ for 1hr in N2 atmosphere. The characterization of the $\beta$-Sialon powder was performed with XRD, BET, SEM and particle size analysis. The sinterability and mechanical properties of the sintered bodies were investigated in terms of bulk density, M.O.R., fracture toughness, morphology of microstructure and etc. The reduction effect of deposited carbon was better than that of activated carbon mechanically added. The formation of SiC was precominant over that of Si2ON2 and $\beta$-Sialon owing to low partial pressure of N2 inside the pore, wehreas on the surface of porous glass the formation of Si2ON2 and $\beta$-Sialon were predominant. Thereafter, SiC reduced unreacted glass to be $\beta$-Sialon. Single phase of $\beta$-Sialon(Z=1.92) was obtained from PGA porous glass having the largest pore radius by the simultaneous reduction and nitridation method at 145$0^{\circ}C$ for 5hrs. The bulk density, M.O.R., and KIC of the sitered body are 3.17g/cc, 434.4MPa and 4.1MPa.m1/2, respectively.