• 한국세라믹학회지
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• 제28권1호
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• pp.11-18
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• 1991

A precipitation method, one of the most effective liquid phase reaction methods, was adopted in order to prepare high-tech Al2O3/ZrO2 composite ceramics, and the effects of stress-induced phase transformation of ZrO2 on thermal shock behavior of Al2O3-ZrO2 ceramics were investigated. Al2(SO4)3.18H2O, ZrOCl2.8H2O and YCl3.6H2O were used as starting materials and NH4OH as a precipitation agent. Metal hydroxides were obtained by single precipitation(process A) and co-precipitation(process B) method at the condition of pH=7, and the composition of Al2O3-ZrO2 composites was fixed as Al2O3-15v/o ZrO2(+3m/o Y2O3). Critical temperature difference showing rapid strength degradation by thermal shock showed higher value in Al2O3/ZrO2 composites(process A : 20$0^{\circ}C$, process B : 215$^{\circ}C$) than in Al2O3(175$^{\circ}C$). The improvement of thermal shock property for Al2O3/ZrO2 composites was mainly due to the increase of strength at room temperature by adding ZrO2. The strength degradation was more severe for the sample with higher strength at room temperature. Crack initiation energies by thermal shock showed higher values in Al2O3/ZrO2 composites than in Al2O3 ceramics due to increase of fracture toughness by ZrO2.

• E2M - 전기 전자와 첨단 소재
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• 제16권9호
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• pp.64.2-65
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• 2003

A 4 nm layer of ZrOx (targeted x-2) was deposited on an interfacial layer(IL) of native oxide (SiO, t∼1.2 nm) surface on 200 mm Si wafers by a manufacturable atomic layer chemical vapor deposition technique at 30$0^{\circ}C$. Some as-deposited layers were subjected to a post-deposition, rapid thermal annealing at $700^{\circ}C$ for 5 min in flowing oxygen at atmospheric pressure. The experimental x-ray diffraction, x-ray photoelectron spectroscopy, high-resolution transmission electron microscopy, and high-resolution parallel electron energy loss spectroscopy results showed that a multiphase and heterogeneous structure evolved, which we call the Zr-O/IL/Si stack. The as-deposited Zr-O layer was amorphous $ZrO_2$-rich Zr silicate containing about 15% by volume of embedded $ZrO_2$ nanocrystals, which transformed to a glass nanoceramic (with over 90% by volume of predominantly tetragonal-$ZrO_2$(t-$ZrO_2$) and monoclinic-$ZrO_2$(m-$ZrO_2$) nanocrystals) upon annealing. The formation of disordered amorphous regions within some of the nanocrystals, as well as crystalline regions with defects, probably gave rise to lattice strains and deformations. The interfacial layer (IL) was partitioned into an upper Si $o_2$-rich Zr silicate and the lower $SiO_{x}$. The latter was sub-toichiometric and the average oxidation state increased from Si0.86$^{＋}$ in $SiO_{0.43}$ (as-deposited) to Si1.32$^{＋}$ in $SiO_{0.66}$ (annealed). This high oxygen deficiency in $SiO_{x}$ indicative of the low mobility of oxidizing specie in the Zr-O layer. The stacks were characterized for their dielectric properties in the Pt/{Zr-O/IL}/Si metal oxide-semiconductor capacitor(MOSCAP) configuration. The measured equivalent oxide thickness (EOT) was not consistent with the calculated EOT using a bilayer model of $ZrO_2$ and $SiO_2$, and the capacitance in accumulation (and therefore, EOT and kZr-O) was frequency dispersive, trends well documented in literature. This behavior is qualitatively explained in terms of the multi-layer nanostructure and nanochemistry that evolves.ves.ves.

• 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.

• 한국세라믹학회지
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• 제32권7호
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• pp.853-857
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• 1995

ZrSiO4 powders were prepared from partially hydrolyzed solution of Si(OC2H5)4 and ZrOCl2.8H2O solution by the sol-gel method and formation rate of ZrSiO4 on the reaction parameter was investigated. In order to prepare homogeneous ZrSiO4 precursor gels, the H2O/Si(OC2H5)4 molar ratio of about 2, the pH of the ZrOCl2.8H2O solution fo about 4 and stirring time of the mixed solutions of about 2 hrs were appropriate. Formation of temperature of ZrSiO4 reduced about 15$0^{\circ}C$ by milling and formation of ZrSiO4 at 1300~135$0^{\circ}C$ showed an accelerative increase through the hedvall effect by silica.

• 한국세라믹학회지
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• 제24권1호
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• pp.33-40
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• 1987

The investigation includes phase equilibria of Al2O3-HfO2 Cr2O3-ZrO2, Cr2O3-HfO2, Al2O3-Cr2O3-ZrO2, Al2O3-Cr2O3-HfO2, Al2O3-ZrO2-HfO2, Cr2O3-ZrO2-HfO2, Al2O3-Cr2O3-ZrO2-HfO2. In the systems the solubility near the end members has been studied at 1500$^{\circ}C$ and 1600$^{\circ}C$, respectively. Selective Compositions were investigated in the area of the guarternary system where the phae relation was examined.

• 공업화학
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• 제17권3호
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• pp.250-254
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• 2006

$Li_{2}ZrO_{3}$의 $CO_{2}$ 제거능을 평가하기 위하여 열중량분석기(thermogravimetric analyser, TGA)를 사용하여 실험하였고 $Li_{2}ZrO_{3}$를 이용한 $CO_{2}$ 제거반응시 $H_{2}$와 CO의 영향을 평가하기 위하여 충전층 반응기를 이용하여 실험하였다. $Li_{2}ZrO_{3}$의 $CO_{2}$ 제거반응 초기속도는 가스유량 증가에 따라 일정하게 증가하였고 가스유량 100 mL/min 이상에서 기체경막저항 소멸에 따라 일정하게 유지되었다. $Li_{2}ZrO_{3}$와 $CO_{2}$의 반응차수는 1차임을 확인했으며 최적온도 구간은 $500{\sim}600^{\circ}C$로 나타났으며, XRD와 SEM을 이용하여 $Li_{2}ZrO_{3}$의 구조를 살펴본 결과 결정구조의 $Li_{2}ZrO_{3}$와 다공성의 $Li_{2}CO_{3}$/$ZrO_{2}$로 구성되어 있음을 확인하였다. 또한 $CO_{2}$ 내의 $H_{2}$ 존재는 $CO_{2}$ 제거반응에 영향을 미치지 않지만 CO의 경우 $Li_{2}ZrO_{3}$상의 $Li_{2}CO_{3}$(L)에 흡착되는 $CO_{2}$의 수착을 억제하는 것으로 나타났다.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2015년도 제49회 하계 정기학술대회 초록집
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• pp.215.1-215.1
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• 2015

본 연구에서는 용액 공정 기반 ZrO2 절연막의 우수한 특성을 확인하기 위해 SiO2 절연막을 가지는 IGZO (Indium-Gallium-Zinc Oxide) 박막 트랜지스터와 비교했다. In:Ga:Zn=1:1:1의 비율의 0.3 M IGZO 용액과 0.2 M ZrO2용액을 사용하였다. ZrO2 박막 트랜지스터는 0.2M ZrO2 용액을 5번 반복 증착하며 140nm 두께의 ZrO2 절연막을 가지는 IGZO 박막 트랜지스터와 비교대상으로 동일한 두께의 SiO2의 절연막을 가지는 IGZO 박막 트랜지스터를 제작하였다. ZrO2 박막 트랜지스터의 문턱전압은 4.3V로 SiO2 박막 트랜지스터의 -6.1V보다 낮았고, 이동도는 $1.2356cm^2/V{\cdot}s$로 $0.0554cm^2/V{\cdot}s$ 보다 약 20배 높았다. 실험 결과를 통해 ZrO2를 절연막으로 사용한 박막 트랜지스터의 특성이 더 향상되었음을 확인하였다.

• 한국세라믹학회지
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• 제42권8호
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• pp.561-566
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• 2005

For the homogeneous dispersion of $ZrO_2$ particles in $Al_2O_3/ZrO_2$ceramics, Zr-precusors were mixed with oxide $Al_2O_3$powders by chemical routes such as partial precipitation or partial polymerization of Zr-nitrate solutions. In case of the mechanical mixing of ultrafine $Al_2O_3$ and $ZrO_2$ oxide powders, relatively homogeneous dispersion was difficult to achieve so that the particle size and distributions of $ZrO_2$ were relatively inhomogeneous after sintering at high temperature. But when the Zr-Y-hydroxide were co-precipitated to ultrafine $Al_2O_3$ oxide powders followed by calcinations, homogeneous dispersion of nano-sized $ZrO_2$ particles in $Al_2O_3/ZrO_2$ composite ceramics were obtained. But because of the coalescence of dispersed $ZrO_2$ particles, dispersed $ZrO_2$ was grown up to more than 0.2${mu}m$ (200 nm) when sintered at the temperature of higher than $1500^{\circ}C$ But when the sintering temperature was kept to lower than $1400^{\circ}C$ by using nano-sized $\alpha-alumina$, the particle size of dispersed $ZrO_2$ could be sustained below 0.1 ${\mu}m$. But the coalescence of dispersed $ZrO_2$ between $Al_2O_3$ particles could not be avoided so that the mechanical properties were not enhanced contrary to the expectations. So Zr-polyester precursors were precipitated and coated to the surface of ultrafine $\alpha-alumina$ powders by the polymerization of Ethylene Glycol with Citric Acid and Zirconium Nitrate. By this dispersion much more uniform dispersion of $ZrO_2$ was achieved at $1450\~1600^{\circ}C$ of sintering temperature ranges. And due to especially discrete dispersion of $ZrO_2$ between $Al_2O_3$ particles, their mechanical strength was more enhanced than mechanical mixing or hydroxide precipitation methods.