• The Korean Journal of Ceramics
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• 제1권3호
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• pp.143-146
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• 1995

Twins along(202) and (211) planes are observed in monoclinic $ZrO_2$ thin film, which is deposited on Si substrate by MOCVD at $350^{\circ}C$ and annealed at $1150^{\circ}C$ for 10 hours in air. These types of twin have not been reported in monoclinic $ZrO_2$. The twins seem to be originated from the two dimensional tensile stresses applied to the $ZrO_2$ thin film due to the different thermal expansions of $ZrO_2$ thin film and Si substrate.

• 한국세라믹학회지
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• 제31권10호
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• pp.1147-1158
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• 1994

From Zr(O-nC3H7)4-H2O-C2H5OH-HNO3 starting solutions, MgO-doped stabilized zirconia fibers with varying content of MgO (10~18 mol%) from different MgO sources were fabricated by sol-gel method. The MgO sources used are magnesium nitrate hexahydrate, magnesium acetate tetrahydrate, and magnesium ethylate. The phase transformation studies of a drawn MgO-ZrO2 fiber were carried out using X-ray diffraction, IR spectroscopy, and Raman spectroscopy. The microstructure, tensile strength, and microporosity of fibers were investigated using SEM, tensile strength test, and microporosimeter. Although various MgO sources such as magnesium nitrate, acetate, and ethylate were used, the crystallization behavior of MgO-ZrO2 fibers at different temperatures could be summarized as follows: CubiclongrightarrowMetastable TetragonallongrightarrowMonocliniclongrightarrowCoexistence of Monoclinic and CubiclongrightarrowCubic(trace of monoclinic). At 150$0^{\circ}C$, the phase transformation of MgO-ZrO2 fibers shows the following change depending on the amount of MgO[Mg(NO3)2.6H2O]: At 10 mol%, both monoclinic and cubic phase coexist, at 12 mol%, monoclinic phase decreases rapidly, and then at 14 mol%, only cubic phase remains. When the MgO-ZrO2 fibers containing 12 mol% magnesium nitrate were heated at 80$0^{\circ}C$ for 1hr, average tensile strength of fibers is 4.0 GPa at diameters of 20 to 30 ${\mu}{\textrm}{m}$. As the heat-treatment temperatures increase to 100$0^{\circ}C$ for 1 hr, tensile strength of MgO-ZrO2 fibers decreases rapidly to 0.7 GPa.

• 한국세라믹학회지
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• 제21권2호
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• pp.149-155
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• 1984

The effect of $ZrO_2$ dispersed phase on the mechanical properties in $Al_2O_3$-$ZrO_2$system has been studied. There are both metastable tetragonal phase and stable monoclinic phase of $ZrO_2$particles diespersed in Al2O3 matrix at room temperature. Metastable tetragonal $ZrO_2$ changes to the stable monoclinic structure within the stress field of the crack. And microcracks are formed by the expansion of $ZrO_2$during the tetragonal-monoclinic transformation on cooling. Therefore stress-induced phase transformation and inclusion-induced microcracking contribute to the mec-hanical properties of $Al_2O_3$-$ZrO_2$system. Sintered composites containing 10m/o $ZrO_2$ yield KiC values of 6.5MN/$m^{3/2}$ much greater than that of pure $Al_2O_3$ This increase results from microcrack extension and stress-induced phase transformation absor-bing energy by crack propagation. Flexural strength of composites is decreased considerably in comparison with pure $Al_2O_3$ This decrease results from microcrack as a crack former and higher porosity than pure $Al_2O_3$.

• Transactions on Electrical and Electronic Materials
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• 제16권2호
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• pp.86-89
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• 2015

Uniform ZrO₂ nanoballs were synthesized at 700℃ using the inverse replication method through a colloid-imprinted carbon (CIC) template. The structural, dielectric, and conducting properties of the ZrO₂ nanoballs were investigated and compared with those of ZrO₂ film prepared by sol-gel method and powdered ZrO₂ chemical. Both the monoclinic and cubic phases were found in the ZrO₂ balls and film but the ZrO₂ chemical showed a monoclinic phase, where the cubic structure is known to be formed at above 2,300℃. ZrO₂ nanoballs showed the lower dielectric property of k = 21.2 at 1 MHz because the 8-coordinated cubic phase in the ZrO₂ nanoball produced lower polarization than the polarization of the 7-coordinated monoclinic ZrO₂ chemical (k = 23.6). The dielectric stability was maintained in each ZrO₂ ball, film, and chemical under the applied forward and reverse voltage range (−5 to +5 V) at 1 MHz. The ionic conductivities were 7.86 × 10⁻⁸/Ω·cm for ZrO₂ nanoballs, 3.29 × 10⁻⁸/Ω·cm for ZrO₂ chemical, and 6.70 × 10⁻⁵/Ω·cm for the thickness of 1,053 nm ZrO₂ film at room temperature with the electronic contribution being less than 0.006%.

• 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.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 1999년도 추계학술대회 논문집
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• pp.335-338
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• 1999

The effect of monoclinic $ZrO_2$(pure) and tetragonal $ZrO_2$ containing 5.35wt% $Y_2$$O_3$(Y-TZP) addition on the mechanical properties and thermal shock resistance of $Al_2$$O_3$ ceramic were investigated. The addition of $ZrO_2$(m) and Y-TZP increased sintering density of $Al_2$$O_3$. The vickers hardness increased with increasing the volume fraction of Y-TZP going through a maximum at 20wt%. The hardness of the specimens was found to be depend on the sintering density. With increasing the volume fraction of $ZrO_2$(m) and Y-TZP, the fracture toughness of the composite is increased. This result may be taken as evidence that toughening of ${Al_2}{O_3}$ can also be achieved by the transformation toughening and microcrack toughening of $ZrO_2$. The property of the& shock for ${Al_2}{O_3}$-$ZrO_2$ composites was improved by increasing the volume fraction of monoclinic $ZrO_2$(pure).Grain size increased with increasing the volume fraction of $ZrO_2$.

• 한국세라믹학회지
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• 제36권12호
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• pp.1390-1395
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• 1999

Zr(Y,Ce)O2 TZP ceramics were prepared by sintering compacts of 3 mol% Y2O3-TZP(3Y-TZP) powders with different amount of 12 mol% CeO2-TZP(12Ce-TZP) in air at 140$0^{\circ}C$ for 2 h. The phase changes microstructure and mechanical properties of Zr(Y. Ce)O2 TZP after hydrothermal aging(20$0^{\circ}C$ 5h) were investigated. Although an addition of 12Ce-TZP accelerated the grain growth of Zr(Y, Ce)O2 TZP it restrained the transformation of tetragonal to the monoclinic phase during aging. The degradation in mechanical properties of sintered bodies was governed by the formed monoclinic phase and chemical composition. Induced Vickers indentation crack was propagated intergranually. From SEM observation of the fracture surfaces the pull-out of individual grain was confirmed.

• 공업화학
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• 제8권2호
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• pp.267-275
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• 1997

본 연구는 졸-겔법을 이용하여 제조한 $ZrO_2$의 하소 온도에 따른 분말특성을 조사하고, 고온수에서 $ZrO_2$의 $Co^{2+}$ 흡착특성을 교반기가 달린 압력용기를 이용한 회분식 흡착 실험으로 알아보았다. 졸-겔법을 이용하여 $ZrO_2$분말을 제조하고, $600{\sim}1400^{\circ}C$로 하소한 후, X-선 회절법, SEM, BET 방법, Fourier transform 적외선 (FT-IR), 열중량 및 열시차분석법(TG-DTA)등을 이용하여 특성 변화를 조사하였다. 비정질의 질코니아는 $480^{\circ}C$부터 tetragonal 질코니아가 생성되고 $600{\sim}1000^{\circ}C$ 온도범위에서는 tetragonal 질코니아와 monoclinic 질코니아가 공존하며, $1200^{\circ}C$에서는 tetragonal 질코니아에서 monoclinic 질코니아로의 상변태가 나타났으며, 고온수에서 하소온도가 $600^{\circ}C$인 $ZrO_2$의 흡착제의 코발트 평형흡착용량은 0.16 meq/g 이었다. $125^{\circ}C$ 이상의 고온에서의 흡착반응은 비가역 흡열반응이며, $600^{\circ}C$에서 하소한 $ZrO_2$의 표준엔탈피 변화값(${\Delta}H^{\circ}$)은 약 18 kJ/gmol 이였다.

• 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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• 제41권2호
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• pp.111-117
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• 2004

고순도 3Y-TZP에 알루미나를 0.3∼l.2wt%까지 첨가하여 attrition milling을 하고 slip-casting하여 시료를 제조하였다. 1390∼151$0^{\circ}C$까지 열처리하여 소결체의 소결특성을 기제적 물성과 미세구조 분석을 통하여 확인하였다. XRD를 이용하여 monoclinic-ZrO$_2$의 생성량을 정량적으로 확인하였으며, 147$0^{\circ}C$ 이장에서 열처리한 시료의 경우 m-ZrO$_2$의 생성으로 밀도의 저하를 보였으며, 비정상 입자성장을 유발하여 경도가 저하되었다. 알루미나의 첨가량이 0.9wt% 미만, 열처리 온도143$0^{\circ}C$에서 microhardness가 1360Hv 이상의 소결체를 제조할 수 있었다.