• Journal of the Korean Crystal Growth and Crystal Technology
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• v.7 no.3
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• pp.377-383
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• 1997

Yttria-stabilized TZP alloyed with pentavalent oxides $(Ta_2O_5,\;Nb_2O_5)$ were fabricated by the conventional sintering method at $1500^{\circ}C$ in air to construct the simplified ternary phase diagram. The phase stability of tetragonal -$ZrO_2$ from the quasi-binary system $ZrO_2-YTa(Nb)O_4$, which do not transform to monoclinic-$ZrO_2$ even for a wide range of grain size and annealing temperature, was investigated to determine composition region of the non-transformable $t-ZrO_2$ solid solution$(NT_{ss})$. Phase stability of $NT_{ss}$ was probably due to the enhanced stability of $_YTa(Nb)O4$ having the tetragonal fergusonite structure. It was experimentally found that mixtures having $NT_{ss}$ alloyed with $T_{ss}$ by weight%% showed both excellent phase stability of $t-ZrO_2$ and fracture toughness even though the calculated composition of the mixture /was located outside $NT_{ss}$ composition region.

• Korean Journal of Materials Research
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• v.30 no.4
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• pp.176-183
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• 2020

The high-temperature stability of YSZ specimens fabricated by die pressure and cold isostatic press (CIP) is investigated in CaCl₂-CaF₂-CaO molten salt at 1,150 ℃. The experimental results are as follows: green density 46.7 % and 50.9 %; sintering density 93.3 % and 99.3 % for die press and CIP, respectively. YSZ foremd by CIP exhibits higher stability than YSZ formed by die press due to denseness dependency after high-temperature stability test. YSZ shows peaks mainly attributed to CaZrO₃, with a small t-ZrO₂ peak, unlike the high-intensity tetragonal-ZrO₂ (t-ZrO₂) peak observed for the asreceived specimen. The t-ZrO₂ phase of YSZ is likely stabilized by Y₂O₃, and the leaching of Y₂O₃ results in phase transformation from t-ZrO₂ to m-ZrO₂. CaZrO₃ likely forms from the reaction between CaO and m-ZrO₂. As the exposure time increases, more CaZrO₃ is observed in the internal region of YSZ, which could be attributed to the inward diffusion of molten salt and outward diffusion of the stabilizer (Y₂O₃) through the pores. This results in greater susceptibility to phase transformation and CaZrO₃ formation. To use SOM anodes for the electroreduction of various metals, YSZ stability must be improved by adjusting the high-density in the forming process.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.10 no.3
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• pp.233-238
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• 2000

t-$ZrO_2/Al_2O_3$composites having a superior biocompatability and phase stability were prepared by adding 0~4 mol% of $Eu_2O_3$and sintered for 1 h at $1600^{\circ}C$ to evaluate phase stability, chromaticity and mechanical properties of the composites. No tetragonal to monoclinic phase transformation was observed for the composites containing $Eu_2O_3$after heat treatment for 20 h at $180^{\circ}C$ under 3.5 MPa water vapor pressure condition. As $Eu_2O_3$content increased, the color of the composites was changed from a slight white ivory to a light pink. The strength and the fracture toughness of the composites containing $Eu_2O_3$were above 620 MPa and 7.6 MPa.$m^{1/2}$, respectively, when $Eu_2O_3$was added up to 3 mol%.

• Journal of the Korean Ceramic Society
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• v.37 no.4
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• pp.354-358
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• 2000

Tetragonal (t)-ZrO2/Al2O3 composites doped with Y2O3, Nb2O5, and Fe2O3 ((Y, Nb, Fe)-TZP/Al2O3) were prepared over the range containing Fe2O3 from 0.1 to 0.5 mol% with 0.1 mol% intervals to evaluate the effect of Fe2O3 addition on chromaticity, hydrothermal stability, and mechanical property of the composites. After autoclaving for 20 h at 18$0^{\circ}C$ under 3.5 MPa water vapor pressure, no tlongrightarrowm phase transformation was observed probably due to the preferential solid solubility of Fe2O3 in Al2O3, the presence of the rigid Al2O3 particles, and the inherent phase stability of (Y, Nb)-TZP. The optimized strength and the fracture toughness of the composite were 700 MPa and 8.5 MPa.m1/2, respectively, when 0.1 mol% Fe2O3 was added. The composites have shown a gradual color change from a slightly white ivory to a pale yellowish brown with increasing the Fe2O3 concentration.

• Journal of the Korean Ceramic Society
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• v.34 no.6
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• pp.645-651
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• 1997

Tetragonal zirconia polycrystals (TZPs) doped with $Y_{2}O_{3}$ and $Nb_{2}O_{5}$ were prepared by the conventional sintering to enhance fracture toughness and phase stability of TZPs without controlling the grain size. TZP composites were obtained by adding the transformable TZP to the non-transformable TZP in wt%. The monolithic tetragonal $ZrO_2$, same as the composite composition containing 15 wt% transformable TZP, sintered at $1550^{\circ}C$ for 10h in air, exhibited the fracture toughness of 9$MPam^{1/2}$ and no low-and high-temperature degradation at temperatures in the range of 220 to $1000^{\circ}C$ for 100h in air. The corresponding single composition was 90.24 mol% $ZrO_2$-5.31 mol% $Y_{2}O_{3}$-4.75 mol% $Nb_{2}O_{5}$. The microstructure observation revealed that the t-$ZrO_2$ grains grew grandually with sintering time and no microcraking and twinning were observed.

• Journal of the Korean Ceramic Society
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• v.33 no.10
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• pp.1177-1185
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• 1996

Y-TZP/Ce-TZP ceramics having relative sintered densities of>95% average grain sizes of 0.36$\mu\textrm{m}$ microhar-dness of 1150 kg/mm2 fracture strength of 390-830 MPa and toughness of 6.4-10.2 MPa$.$mm1/2 were prepared by conventional sintering of 3 mol% Y2O3-ZrO2 and 12 mol% CeO2-ZrO2 powders at 1400 and 1500$^{\circ}C$ The average grain sizes of Y-TZP/Ce-TZP ceramics were mainly governed by those of Ce-TZP. White increasing Ce-TZP content toughness increased while microhardness and fracture strength decreased. With comparing microhardness and toughness fracture strength was more sensitive on not only grain size but also other factors such as microstructural and compositional variations. The densification of Y-TZP/Ce-TZP cermaics was not greatly affected by composition and soaking time at temperature over 1400$^{\circ}C$ With increasing CE-TZP content the stability of t-ZrO2 decreased under thermal aging in air whereas increased in hydrothermal atmosphere and aqueous solution.

• Journal of the Korean Ceramic Society
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• v.32 no.10
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• pp.1147-1161
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• 1995

When ceramic membrance was made from metal salt solution in place of metal akoxide solution, crack free and good adhesion to supporter was optimized for sol stability and good adhesion force. A starting sol was prepared from aluminum oxychloride aqueous solutjion in order to inhibit the grain growthof Al2O3 during heat treatment. The crack free dip coating can't be achieved in 1mol/ι zirconium oxychloride solution because of the high viscosity which interferes with the hydration copolymerization between Al3+ ion and Zr4+ ion. Thus Al2O3-ZrO2 sol stability and viscosity for dip coating was effective when 0.01 mol/ι zirconium oxychloride was added. The minimizing of crack and achieving better adhesion to the supporter wa obtained by microwave drying, surfactant addition and ultrasonic dip coating in wet atmosphere. The result seems to minimize the capillary force and improve the adhesive ability to supporter during the process. Where the average pore size of Al2O3-ZrO2 ultrafilter ceramic membrane measured 17 Å by the BET method and observed γ-Al2O3 phase with tetragonal zirconia after firing at 700℃.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.11 no.4
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• pp.170-175
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• 2001

It was possible to grow the $Al_{2}O_{3}$ based $Y_{3}A_{5}O_{12}(YAG),ZrO_{2}$ binary and ternary eutectic fibers using micro-pulling down method with a growing rate of 0.1~15 mm/min. While $Al_{2}O_{3}/ZrO_{2}$ showed cellular-lamellar structure, $Al_{2}O_{3}$/YAG and $Al_{2}O_{3}$/YAG/$ZrO_{2}$ternary eutectic fibers showed homogeneous Chinese script lamellar structures. The microstructures of $Al_{2}O_{3}/ZrO_{2}$ binary eutectic fibers changed with solidification rate from lamellar pattern to cellular structure. The interlamellar spacing agreed with the inverse-square-root dependance on pulling rate according to $\lambda$=$kv_p\;{-1/2}$. $Al_{2}O_{3}/ZrO_{2}$ binary eutectic fibers recorded the highest tensile strength of about 1560MPa at room temperature. $Al_2O_3/YAG/ZrO_2$ternary eutectic fiber showed excellent thermal stability to $1200^{\circ}C$ without significant decrease. The maximum strength of ternary eutectic fibers recorded were 1100MPa at $25^{\circ}C$ and 970MPa at $1200^{\circ}C$, respectively.

• Korean Journal of Materials Research
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• v.23 no.9
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• pp.531-536
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• 2013

This paper investigates the effect of prolonged high temperature exposure on concentric laminated $Al_2O_3-ZrO_2$ composites. An ultrafine scale microstructure with a cellular 7 layer concentric lamination with unidirectional alignment was fabricated by a multi-pass extrusion method. Each laminate in the microstructure was $2-3{\mu}m$ thick. An alternate lamina was composed of 75%$Al_2O_3$-(25%m-$ZrO_2$) and t-$ZrO_2$ ceramics. The composite was sintered at $1500^{\circ}C$ and subjected to $1450^{\circ}C$ temperature for 24 hours to 72 hours. We investigated the effect of long time high temperature exposure on the generation of residual stress and grain growth and their effect on the overall stability of the composites. The residual stress development and its subsequent effect on the microstructure with the edge cracking behavior mechanism were investigated. The residual stress in the concentric laminated microstructure causes extensive micro cracks in the t-$ZrO_2$ layer, despite the very thin laminate thickness. The material properties like Vickers hardness and fracture toughness were measured and evaluated along with the microstructure of the composites with prolonged high temperature exposure.

• Proceedings of the Korean Ceranic Society Conference
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• 2000.04a
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• pp.48.1-48.1
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• 2000