• The Korean Journal of Ceramics
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• v.1 no.3
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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.

• Journal of the Korean Ceramic Society
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• v.31 no.10
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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.

• Journal of the Korean Ceramic Society
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• v.21 no.2
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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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• v.16 no.2
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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%.

• Journal of the Korean Ceramic Society
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• v.37 no.1
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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.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 1999.11a
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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 $ZrO_2$.

• Journal of the Korean Ceramic Society
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• v.36 no.12
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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.

• Applied Chemistry for Engineering
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• v.8 no.2
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• pp.267-275
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• 1997

$ZrO_2$ Powder was Prepared by sol-gel process and the adsorption characteristic of cobalt($Co^{2+}$) by $ZrO_2$ adsorbent in high-temperature water was investigated using batch adsorption experiment with a stirred autoclave. The prepared $ZrO_2$ was calcined at $600{\sim}1400^{\circ}C$ and analyzed by X-ray diffractometry, SEM, BET surface area, FT-IR and TG-DTA measurement. The tetragonal Phase of $ZrO_2$ is produced $480^{\circ}C$ from amorphous gel at temperature $480^{\circ}C$. Both tetragonal and monoclinic phase of $ZrO_2$ exist at temperature between $600^{\circ}C$ and $1000^{\circ}C$. At temperature $1200^{\circ}C$, tetragonal to monoclinic phase trasition is occurred. The $Co^{2+}$ adsorption capacity of $ZrO_2$ calcined at $600^{\circ}C$ for 4 hours is 0.16 meq $Co^{2+}/g$ adsorbent in the high temperature at $250^{\circ}C$. The adsorption of $Co^{2+}$ on the $ZrO_2$ adsorbent is irreversible endothermic in the temperature range ($125-175^{\circ}C$). The standard enthalpy change (${\Delta}H^{\circ}$) of $ZrO_2$ calcined at $600^{\circ}C$ for 4 hours is 18 kJ/gmol.

• Journal of Industrial Technology
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• v.20 no.A
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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.

• Journal of the Korean Ceramic Society
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• v.41 no.2
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• pp.111-117
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• 2004

3Y-TZP containing 0.3∼1.2 wt% of $Al_2$O$_3$ was prepared by slip-casting after attrition milling. The specimen was sintered at 1390∼151$0^{\circ}C$ and mechanical characterization and microstructure analysis were conducted. Monoclinic content of the specimen was calculated by XRD. The apparent density of specimen increased with increasing sintering temperature. While above 1470%, the formation of m-ZrO$_2$ degraded the density. The microhardness of specimen decreased with temperature because monoclinic phase increased wit the grain growth. The specimen containing $Al_2$O$_3$ below 0.9 wt% sintered at 143$0^{\circ}C$ showed the highest microhardness of 1360 Hv.