• Journal of the Korean Ceramic Society
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• v.39 no.5
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• pp.438-445
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• 2002

In this study, the glass frit of $PbO-TiO-2-SiO_2-BaO-ZnO-Al_2O-3-CaO-B_2O_3-Bi_2O_3-MgO$ system was manufactured. The glass was melted at $1,400{\circ}C$, quenched and attrition-milled. The glass frit powder was pressed and fired for 2h at the range of $750~1,000{\circ}C$. The crystallization of glass frit began at about $750{\circ}$ and at low temperature, the main crystal phases were hexagonal celsian($BaAl_2Si_2O_8$) and alumina. As the firing temperature increased, the crystal phases of monoclinic celsian, zinc aluminate, zinc silicate, calcium titanium silicate and titania appeared. And the increase of firing temperature led to transformation of hexagonal celsian to monoclinic. The only glass frit containing 15wt% PbO had the crystal phase of solid solution of $PbTiO_3-CaTiO_3$. At the frequency of 1 MHz, the dielectric constant of glass frit crystallized was in the range of 11~16 and the dielectric loss less than 0.020. But the glass frit containing 15wt% PbO had the dielectric constant of 17~26 and loss of 0.010~0.015 because of crystal phase of solid solution of $PbTiO_3-CaTiO_3$.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.28 no.2
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• pp.69-73
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• 2018

Crystal growth of ${\alpha}-Fe_2O_3$ nanosized particles of 80~90 nm in size, which were hydrothermally prepared from 0.03 M $FeCl_3$ solution at $100^{\circ}C$, was investigated in Pb-containing and Pb-free frit. By heating ${\alpha}-Fe_2O_3$ nanosized particles in two frits at $800^{\circ}C$, the average diameter of particles in frits was increased to 200~210 nm and 150~160 nm, respectively, and the crystal growth due to the aggregation and sintering of several ${\alpha}-Fe_2O_3$ particles was observed. Formation ratios of larger particles over 100 nm in diameter were 54 % in Pb-free frit and 85 % in Pb-containing frit. After heating ${\alpha}-Fe_2O_3$ particles in frits at $800^{\circ}C$, 7~9 nm in average diameter of pores were formed in particles. Theses pores were derived from the porous structure of original ${\alpha}-Fe_2O_3$ particles and confined in particles during sintering.

• The Korean Journal of Ceramics
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• v.2 no.1
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• pp.33-38
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• 1996

In thick film resistors, the characteristics of the frit and the reaction between glass frit and conductor material play an important role for their electrical properties. In this study, various glass frits in the system of $60RO{\cdot}20SiO_2$ $15B_2O_3{\cdot}5Al_2O_3$(RO=PbO, ZnO, CdO; mole%) were mixed with $RuO_2$ and coated on 96% alumina substrate. Only the glass frit containing PbO was reacted with $RuO_2$in$RuO_{2+}$-thick film resistor and produced the new crystalline phase of $Pb_2Ru_2O_{65}$. Their electrical resistivities strongly depend on the amount of $Pb_2Ru_2O_{65}$ crystalline phase obtained, which varied with firing temperature. The sheet resistivities of these resistors were varied from $10^3\; to\; 10^6\;{\Omega}/{\Box}$ depending on heat treatment, and the absolute value of TCR was decreased as the heat treatment temperature increaed. However, $RuO_2$ did not reacted with the glass frits containing ZnO nor CdO, and the resulting showed very high sheet resistivities.

• Korean Journal of Materials Research
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• v.1 no.4
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• pp.206-213
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• 1991

The crystallized solder glasses with the low melting temperature for electronic package were prepared with the compositions of 77-80wt% PbO, 4.5-6wt% ZnO, 7.5-8.5wt% $B_2O_3$, 1-2wt% CaO, and 0.5-2.0wt% $P_2O_5$ containing 3-7wt% $TiO_2$. The Characterization of the solder glasses were studied using DTA, SEM and XRD. Frit containing 3wt% $TiO_2$ had crytallzation temperature range of $420-440^{\circ}C$. The major crystalline phase was identified as $2PbO{\cdot}ZnO{\cdot}B_2O_3$ by X-ray diffraction. Frits containing 4 wt% $TiO_2$ consisted of crysalline Phases of $PbTiO_3$ and $2PbO{\cdot}ZnO{\cdot}B_2O_3$ in the temperature range of $420-440^{\circ}C$, When g1ass frit containing 5wt% $TiO_2$ were heat-treated in the temperature range of $440-460^{\circ}C$, major crytalline phase was perovskite lead titanate.

• 한국정보디스플레이학회:학술대회논문집
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• 2006.08a
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• pp.1225-1228
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• 2006

In the CNT paste for field emission, PbO frit had a fatal influence on CNTs by accelerating a decomposition of CNTs during firing. In the thermogravimetric analysis on the mixtures of CNTs and other ingredients, it was evident that CNTs began to burn out at ${\sim}350^{\circ}C$ by reacting with PbO. This problem was overcome by replacing the PbO frit by the Pb-free frit such that most of CNTs could survive during firing. Consequently, the emission current of the CNT paste prepared using the lead-free frit was improved as much as 250 %, compared to the PbO-containing one. The CNT paste was further optimized by adding a dispersant, whose dispersibility was assessed by measuring the resistance of the paste. With 10% dispersant added, the emission properties of the paste was greatly enhanced as 50 times higher as those of the paste without a dispersant.

• Journal of the Korean Ceramic Society
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• v.26 no.6
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• pp.829-835
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• 1989

Devitrifing solder glasses in a specific group of glass ceramic materials are extensively used in hermetically sealing alumina electronics packages. Preferred frit glass compositions of this study consist of 37~40wt% PbO, 35~40wt% ZnO, 18~20wt% B2O3, 1~3wt% SiO2, 0~6wt% TiO2. The coated frit glasses crystallize during firing and form a strong hermetic seal. DTA and X-ray diffraction were used to characterize crystallization of the glass frit. Frit seal containing 2wt% TiO2 has crystallization temperature of 550~57$0^{\circ}C$ with surface nucleation. Frit seal containing 6wt% TiO2 has crystallization temperature of 515~5$25^{\circ}C$ with bulk nucleation, and the main crystalline phase was perovskite lead titanate having minus expansion coefficient. The average activation energy for the crystallization calculated from Ozawa equation was 65$\pm$10kcal/mol.

• Journal of the Korean Ceramic Society
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• v.28 no.3
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• pp.215-224
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• 1991

The synthesis of SrTiO3 powders having high purity and homogeneous submicron particle size was attempted by the oxalate method. The microstructure and dielectric properties of SrTiO3 based boundary layer capacitor (BLC) were investigated. Strontium titanyl oxalate[SrTiO(C2O4)2.4H2O] was prepared from the mixing solution of (Sr, Ti) using oxalic acid(H2C2O4) as a precipitating agent at 8$0^{\circ}C$. The crystalline SrTiO3 powder was obtained by thermal decomposition of the precipitate above $600^{\circ}C$. The crystalline SrTiO3 powder containing Nb2O5 as a dopant, TiO2 and SiO2 as additives was sintered at 1360~144$0^{\circ}C$ in the reducing atmosphere to get semiconductive SrTiO3. Insulating material containing PbO-Bi2O3-B2O3 frit was printed on the sintered semiconductive SrTiO3 and fired at 120$0^{\circ}C$ for 2h to get the grain boundary diffusion.

• Journal of the Korean Ceramic Society
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• v.56 no.1
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• pp.71-76
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• 2019

Monochromatic amber phosphor in glasses (PiGs) for automotive LED applications were fabricated with $YAG:Ce^{3+}$, $CaAlSiN_3:Eu^{2+}$ phosphors and Pb-free silicate glass. After synthesis and thickness-thinning process, PiGs were mounted on high-power blue LED to make monochromatic amber LEDs. PiGs were simple mixtures of 566 nm yellow YAG, 615 nm red $CaAlSiN_3:Eu^{2+}$ phosphor and transparent glass frit. The powders were uniaxially pressed and treated again through CIP (cold isostatic pressing) at 200 MPa for 20 min to increase packing density. After conventional thermal treatment at $550^{\circ}C$ for 30 min, PiGs were applied by using GPS (gas pressure sintering) to obtain a fully dense PiG plate. As the phosphor content increased, the density of the sintered body decreased and PiGs containing 30 wt% phosphor had full sintered density. Changes in photoluminescence spectra and color coordination were investigated by varying the ratio of $YAG/CaAlSiN_3$ and the thickness of the plates. Considering the optical spectrum and color coordinates, PiG plates with $240{\mu}m$ thickness showed a color purity of 98% and a wavelength of about 605 nm. Plates exhibit suitable optical characteristics as amber light-converting material for automotive LED applications.

• Journal of the Korean Ceramic Society
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• v.41 no.11
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• pp.851-857
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• 2004

The stabilizing characteristics of heavy metals in the silicate glass (SD), borosilicate glass (BD), and leadsilicate glass (PD) containing Electric Arc furnace (EAF) dust were studied by the Toxic Characterization Leaching Procedure (TCLP) test. Also, the dependence of the amount of EAF dust upon structural changes of SD, BD, and PD glasses and the TCLP results were investigated by the XRD and FT-IR spectroscopy. In the XRD results, all of SD, BD, and PD specimens containing dust up to 30 wt% were amorphous without crystallizing. In the TCLP test, the concentration of heavy metals leached from the glasses increased with the amount of EAF dust added. The SD specimen series showed the lowest heavy metal leaching and the heavy metal leachate of the PD specimens were lower than those of the BD specimens. But, the Pb leaching from the PD specimens was the highest in the PD glass composition due to the high Pb content. The value of oxygen/network former ratio could be used to compare the chemical durability within the same glass series, but not proper to do between the different glass series. Adding the EAF dust to the SD mother glass, decreased the Si-O-Si symmetry and increased the non-bridging oxygen, which weakened the structure and decreased the chemical durability of glasses. In the BD series glasses, the addition of EAF dust caused the structural changes from tetra-borate group to di-borate group and the formation of the 2-dimensional layer structure of pyre- and ortho- borate, which decreased the chemical durability of glasses. It is concluded that SD series glass among the 3 kinds of glasses is the most effective to stabilize the heavy metals of EAF dust.

• Journal of the Korean Ceramic Society
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• v.42 no.2 s.273
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• pp.132-139
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• 2005

Sintering behavior of $BaO-Nd_{2}O_3-TiO_2$ with a Pb-based glassceramics frit were investigated in order to understand an effect of glassceramics as a low temperature sintering agent on dielectric ceramics. A green sheet form was fabricated through tape casting method with the glassceramic fut added $BaO-Nd_{2}O_3-TiO_2$. The dispersion properties, rheological properties and final density of dielectric composit slurry as a function of amount and composition of organic additives was examined. The dispersants' addition was effective in controlling dispersion of the ceramics in solution. The addition of excessive dispersant showed adverse effect on dispersion. The prepared slurries, containing ceramic : powders, glass-ceramics and various kinds of organic viechles, exhibited typical shear thinning behavior. The best properties of tape casting appeared powder to solvent ratio 65 : 35 and amount of the binder 6 wt$\%$ and plasticizer 3 wt$\%$. The viscosity of the slurry was 677 cps and green/sintered density in the tape was $3.3 g/cm^3,\;5.56 g/cm^3$ respectively.