• Journal of the Korean Ceramic Society
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• v.45 no.8
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• pp.459-463
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• 2008

$P_2O_5-SnO_2$ system $0.5SnO_2-xP_2O_5-(0.5-x)B_2O_3$(x=0.1, 0.2, 0.3, 0.4, 0.5) glasses have been prepared for Pb-free low temperature glass frit. A investigation about the effect of $B_2O_3$ substitution on properties of $P_2O_5$ glasses, including glass structure properties, thermal properties, and mechanical properties was presented. Substance that is responsible for in moisture absorption existing circumstances supposes by phosphate, and excess moisture tolerance that state funeral's structure is improved breaking does not affect in state funeral bond that only most single bond remains, and can know that does not suffer big impact in boric oxide anomaly present state. This phenomenon estimates that connect with structure change. It is thought according to link this result the phosphoric acid happened structural change. $B_2O_3$ displacement quantity 0.3 mole put out $BO_4$ structures, but above 0.3 mole it changed with the case $BO_3$ structure which it displaces.

• Journal of the Korean Ceramic Society
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• v.30 no.4
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• pp.289-298
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• 1993

Properties in terms of the variation of the glass compositions, which were density (p), molar volume(Vm), atom/ion packing density (Dp), refractive index (nD), transformation temperature (Tg), dilatometric softening point (Td), thermal expansion coefficient (α), Young's modulus (E), and knoop hardness (KHN) were investigated in CaO-SiO2 glasses and CaO-P2O5-SiO2 glasses containing less than 10mole% of P2O5. Those properties were measured by density measurement kit, Abbe refractometer, dilatometer, ultrasonic pulse echo equipment, and micro hardness tester. When CaO content was increased in CaO-SiO2 glasses, p, Dp, nD, Tg, Td, α, E and KHN were increased, while Vm was decreased. When P2O5 was added to the CaO-SiO2 glasses with constant CaO/SiO2 ratio as 1.07, p, Dp, nD, Tg, Td, α, E and KHN were decreased, while Vm was increased. When the amount of P2O5 in glasses was kept constant, the changes of the properties with variation of CaO content in the CaO-P2O5-SiO2 glasses were very similar to those of CaO-SiO2 glasses. These phenomena could be explained by the structural role of P2O5 in the CaO-P2O5-SiO2 glasses, which was polymerization of siicate structures and resulted in [PO4] monomer structure in glasses. Due to this structural characteristics, the bond strength and packing density were changed with compositions. Proportional relationships between 1) np and Dp, 2) Tg, Td, α and CaO content, 3) E and Vm-1, and 4) KHN and P2O5 content were evaluated in this investigation.

• Journal of the Korean Ceramic Society
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• v.29 no.9
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• pp.729-738
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• 1992

The glass formation and structural change with the glass compositions were investigated in the CaO-P2O5-SiO2 system with less than 40 wt% of P2O5. The glass formation range was determined by XRD, SEM and EDS techniques for water quenched specimens. The structural analyses were made for binary CaO-SiO2 glasses and ternary CaO-P2O5-SiO2 glasses by using FT-IR and Raman spectroscopy. The glass formation was affected by CaO/SiO2 mole ratio, P2O5 content and primary crystalline phase. The stable glass formation range was found when the transformed CaO/SiO2 mole ratio (new factor derived from structural changes) was in the range of 0.72~1.15 with less than 10 mol% of P2O5. The structural analyses of CaO-SiO2 glasses indicated that as the CaO/SiO2 ratio was increased, the nonbridging oxygens in the structural unit of the glasses were increased. With addition of P2O5 to CaO-SiO2 glasses, the P2O5 enhanced the polymerization of [SiO4] tetrahedra unit in CaO-SiO2 glasses, which contained a large portion of nonbridging oxygen. The phosphate eliminated nonbridging oxygens from silicate species, forcing polymerization of silicate structures and produced in [PO4] monomer in glasses. When added P2O5 was kept constant, the structural change with various CaO/SiO2 ratio was very similar to that of CaO-SiO2 glasses.

• Journal of the Korean Ceramic Society
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• v.30 no.6
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• pp.433-440
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• 1993

The bioactivity of glasses in the CaO-SiO2 system and CaO-P2O5-SiO2 system with less than 10mol% of P2O5 was investigated by in vitro test in simulated body flood(SBF). The formation of Ca.P film and hydroxyapatite on the surface of glasses after in vitro test was analysed by X-ray photoelectron spectoscopy (XPS), fourier transform infrared reflection spectroscopy (FT-IRRS), energy dispersive X-ray spectroscopy (EDS), and scanning electron microscopy (SEM) observation. In the early stage of Ca.P film formation after in vitro test for CaO-SiO2 and CaO-P2O5-SiO2 glasses, the rate of Ca.P film formation on the surface of the glasses was dependent of structural parameter (Y) evaluated from the glass composition. First, in the case of the glasses having Y value below 2, Ca.P film and SiO2-rich layer were formed simultaneously, and there were no differences of the rate of Ca.P film formation in terms of the Y values. Second, in the case of the glasses having Y value above 2, the SiO2-rich layer was formed, and then Ca.P.Si mixed layer was formed in the silica gel structure of the SiO2-rich layer, and finally the Ca.P film on the surface of SiO2-rich layer. The rate of Ca.P film formation delayed as the Y values increased. The rate of hydroxyapatite formation of glasses (the rate of transformation from Ca.P film to hydroxyapatite) seems to be propotional to the rate of Ca.P film formation and Y value. The rate of hydroxyapatite formation of glasses belonging to the second group was delayed as structural parameter increased, and the hydroxyapatite crystal showed spherical growth in the early reaction stage, and then showed silkworm-like linear growth as the reaction time increased.

• Journal of the Korean Ceramic Society
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• v.30 no.7
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• pp.535-542
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• 1993

It was investigated in this study that a preparation method, activation energy, surface area, pore volume, pore size distribution and DTA analysis of the dry gel in process of producing monolithic porous gel in Li2O-Al2O3-TiO2-SiO2 system by the sol-gel technique using metal alkoxides. Activation energy for gellation according to the variation of water concentration and the kind of catalysts ranged from 10 to 20kcal/mole. Monolithic dry gels were prepared after drying at 9$0^{\circ}C$ when the amount of water for gellation was 4~8 times more than the stoichiometric amount, that was necessary for the full hydrolysis of the mixed metal alkoxide. The specific surface area, the pore volume, the average pore radius of the dried gel at 18$0^{\circ}C$ according to the various kinds of catalyst were about 348~734$m^2$/g, 0.35~0.70ml/g and 10~35$\AA$, respectively. It showed that the dry gels were porous body. As a result ofthe analysis of DTA, it was confirmed that the exothermaic peaks at 715$^{\circ}C$ and 77$0^{\circ}C$ was clue to the crystallization of dried gel.

• Journal of the Korean Ceramic Society
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• v.31 no.10
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• pp.1218-1230
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• 1994

In manufacturing process of porous glass-ceramics by the filler method, the sintering behaviour of crystallizable glass powder mixed with various salts was studied and also the effects of precipitated crystal phases on the properties of porous glass-ceramics were investigated. Fine-grained crystallizable glass powder was homogeneously mixed with various slat having grain size 100~200 ${\mu}{\textrm}{m}$ and sintered for densification. After washing out the inorganic salt with distilled water, the porous sintered body was heat treated additionly for crystallization. The MgO-Al2O3-SiO2 base glass was used as crystallizable glass powder and the water soluble salts such as K2SO4 and MgSO4 were used as filler. When K2SO4 was used, leucite crystal phase was formed as a result of the ion exchange and porous glass-ceramics which exhibit high temperature resistance and high thermal expansion coefficient of 17$\times$10-6/$^{\circ}C$ could be obtained. On the contrary, when MgSO4 was used, only slight ion exchange is observed and $\mu$-cordierite and $\alpha$-cordierite crystal phases were formed and porous glass-ceramics which exhibit low thermal expansion coefficient schedule were determined with the results of DTA curves, thermal shrinkage curves and XRD patterns analysis. From DTA curves and thermal shrinkage curves, it was found that the sintering densification have been completed at the temperature range of exothermic peak for crystallization. The pore size distributions and pore diameters were measured by mercury porosimeter. The pore diameter of porous glass-ceramics was 10~15 ${\mu}{\textrm}{m}$ when 100~200${\mu}{\textrm}{m}$ grain size of K2SO4 was used and it was 25~30 ${\mu}{\textrm}{m}$ when the same grain size of MgSO4 was used. The porous glass-ceramics K2SO4 used shows bimodal pore size distribution and its porous skeleton structure was ascertained by SEM observation.

• Journal of the Korean Ceramic Society
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• v.31 no.7
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• pp.695-702
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• 1994

Current study was undertaken to explain the structural evolution and corresponding changes in the properties of calcium aluminate glasses with the variation of SiO2 doping concentration. Calcium aluminate glasses in the compositional ranges of (100-x)(0.6CaO+0.4Al2O3)+xSiO2(where x=0~60) were fabricated. DTA analysis confirmed an anomalous behavior in glass transition temperature (Tg) with the maximum of 887$^{\circ}C$ and minimum of 859$^{\circ}C$ when x=5 and 50, respectively. densities and refractive indices monotonically decreased with increasing SiO2 content and IR transmitting cutoff shifted to shorter wavelength side when the amount of added SiO2 exceeded 5 mole%. IR fundamental vibration absorption peaks showed the change that NBOs were inclined to SiO4 tetrahedron in the low-silica region and NBO per SiO4 tetrahedra changed from 2 to 0 with increasing silica content. Based on the analysis of IR fundamental vibration absorption peaks, the model of the structural change can be proposed in three step: 1) SiO4 scavenged the NBOs located at AlO4-tetrahedra, which resulted in the increased of Tg values, 2) NBOs located in the main network again with a decrease in Tg, and 3) dominated by the decrease in the relative amount of NBOs in the glass system, where Tg re-increased.

• Journal of the Korean Ceramic Society
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• v.18 no.1
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• pp.13-22
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• 1981

This study is to investigate the effective mineralizer in the manufacture of forsterite porcelain as a high frequency insulator. A mixture of $Mg(OH)_2$. and $SiO_2$.($\alpha$-Quartz) corresponding to the molar ratio of 2.0 MgO: 1.0 $SiO_2$ was prepared from the materials of high purity. It was heated to 140$0^{\circ}C$ at the rate of 20$0^{\circ}C$/hr, which was kept constantly for 1 hour, and one has made chamotte after cooling. Six kinds of glasses were prepared by an 0.1 atomic equivalent of K ions substitution-Ba, Bi, Zn, Cd, Zr-to the basic K-glass (0.333 $K_2O$.1.14 $SiO_2$) and were melted approximately at 150$0^{\circ}C$. The forsterite bodies were provided by adding each glass (10, 15, 20, 25, 30%) to the forsterite chamotte, which was fired at 1320, 1360, 1400, 144$0^{\circ}C$. (1 hr). One has examined the physical and dielectric properties for the specimens. The results of the experiments are as follows; 1. As for water absorption: Bodies were better vitrified with an addition and temperature change of Ba, Bi, Zn-glasses. The specimen containing Cd-glass showed deviation of slow decreasing, where as K-glass was completely not vitrified. 2. Bodies containing Ba, Zn, Bi-glasses appeared comparatively high Modulus of Rupture at 136$0^{\circ}C$, while containing Zr-glass had the highest Modulus of Rupture as the addition changes remarkably at 140$0^{\circ}C$. 3. It was estimated that 20-25% glass present in a forsterite bodies were in good conditions as for physical properties. 4. Specimens of Ba, Bi, Zr-glasses were superior as for dielectric properties, where among Ba-glass was most excellent. 5. Dielectric constant commonly increases in a slight gradient as firing temperature rises. 6. The petrographic examination showed that the bodies containing Ba, Bi-glasses had fine crystals, and were observed distinctly large mosaic crystals in the Zn-glass.

• 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.47 no.2
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• pp.117-121
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• 2010

$SnO_2-(1-x)P_2O_5-xB_2O_3$ glass system were prepared by melt-quenching technique in the compositional series containing 50, 55 and 60 mol% of $SnO_2$. Local structure of the glasses was investigated by Raman and FT-IR measurements. A large glass-forming region was found at the phosphate side of the ternary system with homogeneous glasses containing up to 5~25 mol% of $B_2O_3$. According as content of $B_2O_3$ increases, theraml expansion coefficient of glass decreased but transition temperature and softening temperature increased. Because these phenomenon changed local structure of glass. According as content of $B_2O_3$ increases, quantity of bridging oxygen increased. Also, according as content of $SnO_2$ increases, confirmed that quantity of non-bridging oxygen increases.