• 한국세라믹학회지
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• 제32권5호
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• pp.617-625
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• 1995

In order to reduce reflectance of soda-lime glass having average reflectance of 7.35% and refractive index of 1.53, single (SiO2), double (SiO2/20SiO2-80ZrO2), and triple (SiO2/ZrO2/75SiO2-25ZrO2) layers were designed and fabricated on the glass substrate by Sol-Gel method. Stble sols of SiO2-ZrO2 binary system for antireflective (AR) coatings were synthesized with tetraethyl orthosilicate (TEOS) and zirconium n-butoxide as precursors and ethylacetoacetate (EAcAc) as a chelating agent in an atmosphere environment. Films were deposited on soda-lime glass at the withdrawal rates of 3~11 cm/min using the prepared polymeric sols by dip-coating and they were heat-treated at 45$0^{\circ}C$ for 10 min to obtain homogeneous, amorphous and crack-free films. In case of SiO2-ZrO2 binary system, refractive index of film increased with an increase of ZrO2 mol%. Designed optical constant of films could be obtained through varying the withdrawal rate. In the visible region (380~780nm), reflectance was measured with UV/VIS/NIR Spectrophotometer. Average reflectances of the prepared single-layer [SiO2 (n=1.46, t=103nm)], double-layer [SiO2 (n=1.46, t=1-4nm)/20SiO2-80ZrO2 (n=1.81, t=82nm)], and triple-layer [SiO2 (n=1.46, t=104nm)/ZrO2 (n=1.90, t=80nm)/75SiO2-25ZrO2 (n=1.61, t=94 nm)] were 4.74%, 0.75% and 0.38%, respectively.

• 한국세라믹학회지
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• 제34권7호
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• pp.774-780
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• 1997

Porous low reflective coating films of SiO2.ZrO2 system were prepared from the mixed alkoxide solutions of Zr(O-nC3H7)4 and partially prehydrolyzed TEOS by the sol-gel method using the dip-coating technique. In the case of 90SiO2.10ZrO2 porous coating films with HCl and H2O content was 0.3 mole and 4 mole, 378 m2/g of the specific surface area, 0.254 cm3/g of total pore volume, 30-50$\AA$ of average pore diameter. The transmittance of 90SiO2.10ZrO2 porous coated films was 95.38% at the wavelength of 550 nm, compared with the parent glass, the transmittance was increased with 4.38%.

• 한국세라믹학회지
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• 제37권1호
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• pp.50-56
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• 2000

Precursor gels with the composition of xZrO2·(100-x)SiO2 systems (x=10, 20 and 30 mol%) were prepared by the sol-gel method. Kinetic parameters, such as activation energy, Avrami's exponent, n, and dimensionality crystal growth value, m, have been simultaneously calculated from the DTA data using Kissinger and Matusita equations. The crystallite size dependence of tetragonal to monoclinic transformation of ZrO2 was investigated using XRD, in relation to the fracture toughness. The crystallization of tetragonal ZrO2 occurred through 3-dimensional diffusiion controlled growth(n=m=2) and the activation energy for crystallization was calculated using Kissinger and Matusita equations, as about 310∼325±10kJ/mol. The growth of t-ZrO2, in proportion to the cube of radius, increased with increasing heating temperature and hteat-treatment time. It was suggested that the diffusion of Zr4+ ions by Ostwald ripening was rate-limiting process for thegrowth of t-ZrO2 crystallite size. The fracture toughness of xZrO2·(100-x)SiO2 systems glass ceramics increased with increasing crystallite size of t-ZrO2. The fracture toughness of 30ZrO2·70SiO2 system glass ceramics heated at 1,100℃ for 5h was 4.84 MPam1/2 at a critical crystaliite size of 40 nm.

• Journal of Ceramic Processing Research
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• 제19권6호
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• pp.504-508
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• 2018

Diopside is a ceramic material with excellent physical and chemical properties. However, when it is applied as an LED packaging material, heat dissipation of the LED element is not sufficient due to its relatively lower thermal conductivity, which may cause degradation of the LED function. In this study, glass-ceramics based on a $ZrO_2-CaO-MgO-SiO_2$ system, in which diopside is the main crystal phase, were prepared by heat-treating the glass, which was composed of zircon ($ZrO_2-SiO_2$) powders and diopside ($CaO-MgO-2SiO_2$) powders. The possibility of using the glass-ceramics as a packaging material for LEDs was then investigated by analyzing the density, shrinkage, thermal conductivity, and phases generated according to the amount of zircon powder added. The density and shrinkage of specimens decreased slightly and then increased again with the amount of $ZrO_2-SiO_2$ added within a range of 0~0.38 mol. Even though the crystal phase of zircon does not appear in the $ZrO_2-CaO-MgO-SiO_2$ system, the glass containing 0.38 mol zircon powder showed the highest thermal conductivity, 1.85 W/mK, among the specimens fabricated in this study: this value was about 23% higher than that of pure diopside. It was found that the thermal conductivity of the glass-ceramics based on a $ZrO_2-CaO-MgO-SiO_2$ system was closely related to the density, but not to the phase type. Zirconia ($ZrO_2$), a component oxide of zircon, plays an important role in increasing the density of the specimen. Furthermore the thermal conductivity of glass-ceramics based on a $ZrO_2-CaO-MgO-SiO_2$ system showed a nearly linear relationship with thermal diffusivity.

• 한국세라믹학회지
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• 제29권3호
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• pp.223-231
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• 1992

CaO and ZnO were added to Al2O3-SiO2 binary system respectively as flux, then ZrO2 and TiO2 were applied as nucleating agent to these CaO-Al2O3-SiO2 and ZnO-Al2O3-SiO2 ternary system glass. The transparency could not be kept in CaO-Al2O3-SiO2 system glass, whereas the transparent glass-ceramics were prepared in ZnO-Al2O3-SiO2 system glass containing ZrO2 as the nucleating agent. At this time the optimum heating temperatures for the nucleation and the crystal growth were 78$0^{\circ}C$ and 97$0^{\circ}C$. The sizes of the precipitated crystals in the transparent glass-ceramics were below 0.1 ${\mu}{\textrm}{m}$, and their light transmissibilities were more than 80%.

• 공업화학
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• 제5권6호
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• pp.1044-1055
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• 1994

Ar 또는 $Ar/H_2$ 가스유통(100~500ml/min)하에서 $ZrSiO_4/C$계 및 $ZrSiO_4/Al/C$계로부터 ZrC/SiC 복합분체의 합성을 $1600^{\circ}C$ 온도범위 내에서 시도하고, 이의 생성기구, 생성속도 및 분체특성을 검토하였다. $ZrSiO_4/C$계에서는 $1400^{\circ}C$ 이상에서 $ZrO_2(s)$와 SiO(g)가 각각 탄소와 경쟁반응하여 ZrC 및 SiC를 생성하였다. ZrC생성을 위한 겉보기활성화에너지는 약 18.5kcal/mol($1400-1600^{\circ}C$)이었다. 한편 $ZrSiO_4/Al/C$계에서는 $1200^{\circ}C$ 이상에서 ZrO(g)가 Al(l, g) 및 탄소와 반응하여 ZrC를 생성하였으며, $1300^{\circ}C$ 이상에서는 SiO(g)가 Al(l, g) 및 탄소와 환원-탄화반응하여 SiC를 생성하였다. $1600^{\circ}C$, 5시간 반응으로 얻은 생성물은 평균입경 $21.8{\mu}m$을 갖는 분말로서 ZrC의 격자정수는 $4.679{\AA}$, 결정자크기는 $640{\AA}$이었으며 SiC의 격자정수는 $4.135{\AA}$, 결정자크기는 $540{\AA}$ 정도이었다.

• 산업기술연구
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• 제20권A호
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• pp.247-256
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• 2000

Precursor gels with the composition of $xZrO_2{\cdot}(100-x)SiO_2$ systems (x=10, 20 and 30 mol%) were prepared by the sol-gel method. Kinetic parameters, such as activation energy, Avrami's exponent, n, and dimensionality crystal growth value, m, have been simultaneously calculated from the DTA data using Kissinger and Matusita equations. The crystallite size dependence on tetragonal to monoclinic transformation of $ZrO_2$ was investigated using XRD, in relation to the fracture toughness. The crystallization of tetragonal $ZrO_2$ occurred through 3-dimensional diffusion controlled growth(n=m=2) and the activation energy for crystallization was calculated using Kissinger and Matusita equations, as about $310{\sim}325{\pm}10kJ/mol$. The growth of $t-ZrO_2$, in proportion to the cube of radius, increased with increasing heating temperature and heat-treatment time. It was suggested that the diffusion of Zr4+ions by Ostwald ripening was rate-limiting process for the growth of $t-ZrO_2$ crystallite size. The fracture toughness of $xZrO_2{\cdot}(100-x)SiO_2$ systems glass ceramics increased with increasing crystallite size of $t-ZrO_2$. The fracture toughness of $30ZrO_2{\cdot}70SiO_2$ system glass ceramics heated at $1,100^{\circ}C$ for 5 h was $4.84Mpam^{1/2}$ at a critical crystaliite size of 40 nm.

• 한국세라믹학회지
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• 제28권8호
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• pp.635-639
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• 1991

Monolithic gels in the ZrO2-SiO2 system containing up to 30 mol% ZrO2 were prepared from the mixed solutions of Zr(O.nC3H7)4 and partially prehydrolyzed Si(OC2H5)4 (Tetraethyl orthosilicate) by the sol-gel method. The effect of parameters such as the hydrolysis temperature, the amount of water and HCl on the hydrolysis condensation process was investigated and the obtained gels were studied by the IR spectra and TG-DTA. The results showed that the gelation time becomes shorter with increasing content of HCl, H2O and gelation temperature, and that the polymerization was more easily completed with the higher water volume causing the elimination of unreacted organic groups.

• 한국세라믹학회지
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• 제31권8호
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• pp.934-940
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• 1994

Fibers of ZrO2-SiO2 system were prepared from the hydrolysis and condensation of Si(OC2H5)4 and Zr(OnC3H7)4 with different H2O/alkoxide molar ratios. It was found that fibers could be drawn in the viscosity range of 1~100 poise from HCl catalyzed solutions with lower water contents of the mole ratio H2O/alkoxide, r 2. The fibrous gels were converted into the corresponding oxide glass fibers by heating at 80$0^{\circ}C$. Mechanical test was performed on E, A and 20ZrO2-80SiO2 glass fibers reinforced cement in order to investigate the flexural strength. The flexural strength value of 20ZrO2-80SiO2 glass fibers reinforced cement was greater than those of E and A. The chemical durability of the fibers in alkaline solutions increased with ZrO2 content. The weight loss due to the corrosion by 2N-NaOH solutions at $25^{\circ}C$ for 160 hours was about 0.31$\times$10-2 mg/dm2 for the 20ZrO2-80SiO2 glass fibers, which was superior to that of Vycor glass.

• 한국세라믹학회지
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• 제23권3호
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• pp.87-93
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• 1986

Yttria-bismuth-stabilized zirconia was investigated with respect to the amount of $Bi_2O_3$ addition in the ran-ge of 0.5~5mol% to the base composition of $(ZrO_2)_{0.92}(Y_2O_3)_{0.08}.Bismuth was introduced into the ma-terial with $Bi_2O_3-SiO_2$ glasses in order to reduce the evaporation of components. The sinterbility evaporation of components phase formation and microstructure were evaluated depending on the amount of $Bi_2O_3-SiO_2$ glass addition. Two probe A. C conductivity measurement was subjected to all the specimens and the result was discussed on the possible substitution of $Bi^{3+}$ for $Zr^{4+}$ and interistial $Si^{4+}$ in the fluorite structure of zirconia crystal there-upon the possible change in the capability of oxygen transference within the material. It was found that the addition of $Bi_2O_3$ could improve the sinterbility of material very much while not so much.oxygen sensing material suitable for relative low temperature firing.