• 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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• 제34권6호
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• pp.577-582
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• 1997

The mechanical properties of Al2O3-ZrO2 composites fabricated by RBAO(reaction bonded aluminium oxide) process were investigated. As the amount of ZrO2 increased the sinstered density of Al2O3-ZrO2 composites decreased slightly, but wear resistance was enhanced. Bending strength of Al2O3-ZrO2 composites increased in proportion to the amount of al in case of a fixed ZrO2 content. When the amount of Al was fixed bending strength reached its maximum value at 25 wt% ZrO2. The fracture toughness(K1c) increased with increasing content of ZrO2, but decreased with increasing Al amount. On the other hand, the fracture mode of Al2O3-ZrO2 composites was the mixed mode of inter-and transgranular fracture.

• 한국세라믹학회지
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• 제34권2호
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• pp.145-156
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• 1997

2성분계(CaO-, Y2O3-, MgO-ZrO2) 및 3성분계(MgO-ZrO2-Al2O3)ZrO2분말의 안정화제 종류, 첨가량 및 열처리온도 변화에 따른 ZrO2의 상전이를 X-선 회절과 Raman분광법으로 연구하였다. CaO-, 및 Y2O3-ZrO2계에서 CaO와 Y2O3의 첨가량이 각각 6~15mol% 및 3~15mol%로 증가에 따른 정방정상에서의 입방정상으로의 상전이를 X-선회절 pattern으로는 판별하기 어려웠으나, Raman spectra에서는 모든 Raman band가 저파수쪽으로 이동하고 band의 수 및 그 세기가 현저히 감소함을 관찰할 수 있었다. 이것은 정방정$\longrightarrow$입방정의 상전이가 발생한 것으로 ZrO2 격자내에서 Zr4+ 이온과 Ca2+ 혹은 Y3+이온의 치환에 의해 산소이온의 빈자리 생성으로 인한 구조적 불규칙성과 선택규칙(k=0)의 파괴에 기인한 것으로 해석된다. MgO의 경우에는 10mol%에서 단사정에서 입방정으로 상전이가 발생하였다. MgO-ZrO2-Al2O3계에서는 Al2O3의 첨가에 의해 입방정$\longrightarrow$단사정의 상전이가 발생하는데 이것은 MgO와 Al2O3의 반응에 의해 spinel(MgAl2O4)의 형성으로 인하여 MgO가 충분히 안정화제로서의 역할을 하지 못하기 때문으로 판단된다. 또한, 안정화제의 종류와 첨가량 변화에 따른 ZrO2의 상전이를 ZrO2의 격자상수값의 변화와 관련하여 설명할 수 있는데, 즉, 안정화제의 첨가량이 증가할수록 격자상수 a값은 증가하고 c값은 감소하여 10~13mol%사이에서는 c/a의 축비가 1에 근접하고, 따라서 정방정$\longrightarrow$입방정의 상전이가 진행됨을 알 수 있었다.

• 한국재료학회지
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• 제24권5호
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• pp.259-265
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• 2014

$ZrO_2$ films were coated on aluminum etching foil by the sol-gel method to apply $ZrO_2$ as a dielectric material in an aluminum(Al) electrolytic capacitor. $ZrO_2$ films annealed above $450^{\circ}C$ appeared to have a tetragonal structure. The withdrawal speed during dip-coating, and the annealing temperature, influenced crack-growth in the films. The $ZrO_2$ films annealed at $500^{\circ}C$ exhibited a dielectric constant of 33 at 1 kHz. Also, uniform $ZrO_2$ tunnels formed in Al etch-pits $1{\mu}m$ in diameter. However, $ZrO_2$ film of 100-200 nm thickness showed the withstanding voltage of 15 V, which was unsuitable for a high-voltage capacitor. In order to improve the withstanding voltage, $ZrO_2$-coated Al etching foils were anodized at 300 V. After being anodized, the $Al_2O_3$ film grew in the directions of both the Al-metal matrix and the $ZrO_2$ film, and the $ZrO_2$-coated Al foil showed a withstanding voltage of 300 V. However, the capacitance of the $ZrO_2$-coated Al foil exhibited only a small increase because the thickness of the $Al_2O_3$ film was 4-5 times thicker than that of $ZrO_2$ film.

• 한국세라믹학회지
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• 제28권1호
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• pp.53-59
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• 1991

The reaction product between Si3N4 and ZrO2 has been studied by heat treatment of Si3N4-Zr(Y)O2 composite in high vacuum(<10-5 torr) and in air at $700^{\circ}C$. ZrN was formed after heat treatment in vacuum and easily oxidized after heat treatment in air. The amount of ZrN is related to the Y2O3 content dissolved in ZrO2. After the heat treatment in air the toughness increased and the spalling due to the oxidation of ZrN in specimen surface was observed. As a result, it is suggested that the formation of ZrN phase in Si3N4-ZrO2 composite enhance the toughness of the composite in an oxidation conditon.

• 한국세라믹학회지
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• 제48권1호
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• pp.69-73
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• 2011

A $ZrO_2$ thin film as a corrosion protective layer was deposited on Zircaloy-4 (Z-4) clad material using $N_2O$ as a reactive gas by RF reactive magnetron sputtering at room temperature. The Z-4 substrate was located in plasma or out of plasma during the $ZrO_2$ deposition process to investigate mechanical and corrosive properties for the plasma immersion. Tetragonal and monoclinic phases were existed in $ZrO_2$ thin film immersed in plasma. We observed that a grain size of the $ZrO_2$ thin film immersed in plasma state is larger than that of the $ZrO_2$ thin film out of plasma state. In addition, the corrosive property of the $ZrO_2$ thin films in the plasma was characterized using the weight gains of Z-4 after the corrosion test. Compared with the $ZrO_2$ thin film immersed out of plasma, the weight gains of $ZrO_2$ thin film immersed in plasma were larger. These results indicate that the $ZrO_2$ film with the tetragonal phase in the $ZrO_2$ can protect the Z-4 from corrosive phenomena.

• 한국세라믹학회지
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• 제34권6호
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• pp.583-590
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• 1997

The effects of Mn2O3 and Y2O3 additives on the microstructure and dielectric properties of Sr(Zr, Ti)O3 have been investigated. Powders with Sr(Zr1-xTix)O3(0$\leq$x$\leq$0.1) composition were prepared by the conventional solid state processing from commercial TiO2 and precipitation-processed ZrO2. The powders containing sintering additives of Mn2O3 and Y2O3 were compacted and then sintered at 1,55$0^{\circ}C$ for 4 h to get>97% relative density. Mn2O3 suppressed the grain growth and Y2O3 enhanced the density of sintered body. The oxidation state of Mn ions were determined by a chemical wet method and EPR spectroscopy. Mn ions were present as Mn2+ and Mn4+ in SrZrO3, while as Mn3+ and Mn4+ in Ti-substituted Sr(Zr, Ti)O3. With the substitution of Ti, the lattice parameters of SrZrO3 decreased and its dielectric constant increased with remarkable decrease in Q value. The dielectric constant of Sr(Zr, Ti)O3 was in the range of 30 to 40, Q values 1,200~5,400 at 6 GHz and temperature coefficient of resonant frequency -67~100 ppm/K.

• 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.

• 분석과학
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• 제13권6호
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• pp.712-721
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• 2000

$LiF-BeF_2-ZrF_4$(63-30-7 mol%) 용융염은 상온에서 증류수 1ml당 최고 0.02g까지 용해율 99.9%로 용해되었다. 그리고 $ZrF_4$를 열가수분해시켜 제조된 $ZrO_2$ 산화물을 포함하는 $LiF-BeF_2-ZrF_4$ 용융염에서 $ZrO_2$ 산화물을 증류수로 침출시켜 회수하였다. 회수된 $ZrO_2$ 산화물의 결정모양은 손상되지 않았다.

• 소성∙가공
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• 제7권5호
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• pp.481-488
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• 1998

The active metal brazing was applied to bond Alumina and Ni-Cr steel by Ag-Cu-Zr-Sn alloy and the interfacial microstructure and reaction mechanism were investigated. Polycrystalline monoclinic $ZrO_2$ with a very fine grain of 100-150 nm formed at the alumina grain boundary contacted with Zr segregation layer at the interface. The $ZrO_2$ layer containing the inclusions and cracks were developed at the boundary of inclusion/$ZrO_2$ due to the difference in specific volume. The development of $ZrO_2$ at the interface was successfully explained by the preferential penetration of $ZrO_2$ at the interface was successfully explained by the preferential penetration of Zr atoms a higher concentration of oxygen and a high diffusion rate of Al ions into molten brazing alloy.