• Journal of the Korean Ceramic Society
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• v.27 no.2
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• pp.233-243
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• 1990

For theinvestigation of MgO addition effect on 12Ce-TZP ceramics, MgO-CeO2-ZrO2 ceramics was fabricated using commercial powders under sintering condition of 130$0^{\circ}C$-1$600^{\circ}C$ for 2hr. Fully tetragonal phase could be obtained by proper heat treatment and MgO addition amount. Minor cubic phase was appeared in relatively high MgO content composition at each sintering temperature. As alloying amount of MgO increased, tetragonal stability increased and grain size decreased. Grain size dependence on MgO content was verified by SEM observation of fractured surface. Surface bloating was observed from the 2 m/o to 6m/o in the temperature range of 150$0^{\circ}C$ to 1$600^{\circ}C$. In spite of very porous microstructure owing to surface bloating, 100% TZP could be maintained in 2.0m/o MgO composition by heat treatment of 150$0^{\circ}C$. This result indicated that MgO was more powerful stabilizer than CeO2. Mechanical proprties of MgO-CeO2-ZrO2 ceramics were consistent with the stability observation of tetragonal phase very well.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.24 no.4
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• pp.140-144
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• 2014

Co-(0.7 wt%) and Pr-(2.0, 3.5 or 5.0 wt%) doped cubic zirconia ($ZrO_2:Y_2O_3=50:50wt%$) single crystals grown by a skull melting method were heat-treated in $N_2$ at $1150^{\circ}C$ for 5 hrs. The brown colored as-grown single crystals were changed into either dark brownish green, greenish blue and light green color after the heat treatment. Before and after the heat treatment, the YSZ (yttria-stabilized zirconia) single crystals were cut for wafer form (${\phi}7.5mm{\times}t3mm$). The optical and structural properties were examined by UV-VIS spectrophotometer and X-ray diffraction. Absorption by $Co^{2+}$(${\fallingdotseq}589nm$: ${\Gamma}_8[^4A_2(^4F)]{\rightarrow}{\Gamma}_8+{\Gamma}_7[^4T_1(^4F)]$, ${\fallingdotseq}610nm$: ${\Gamma}_8[^4A_2(^4F)]{\rightarrow}{\Gamma}_8[^4T_1(^4F)]$], ${\fallingdotseq}661nm$: ${\Gamma}_8[^4A_2(^4F)]{\rightarrow}{\Gamma}_6[^4T_1(^4F)]$]) and $Pr^{3+}$(${\fallingdotseq}450nm$: ${^3}H{_4}-{^3}P{_2}$, ${\fallingdotseq}473nm$: ${^3}H{_4}{\rightarrow}{^3}P{_1}$, ${\fallingdotseq}484nm$: ${^3}H{_4}{\rightarrow}{^3}P{_0}$), change of ionization energy and lattice parameter were confirmed.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.22 no.2
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• pp.73-77
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• 2012

Co-(0.8 wt%) and Ce-(0.4 wt%) doped cubic zirconia ($ZrO_2$ : $Y_2O_3$ = 80 : 20, 70 : 30, 60 : 40, 50 : 50 wt%) single crystals grown by a skull melting method were heat-treated in $N_2$ at $1000^{\circ}C$ for 5 hrs. The orange, yellowish brown and brown colored as-grown single crystals were changed into either brownish red, yellow and green color after the heat treatment. Before and after the heat treatment, the YSZ (yttria-stabilized zirconia) single crystals were cut for wafer form (${\phi}6.5mm{\times}t2mm$). The optical and structural properties were examined by UV-VIS spectrophotometer and X-ray diffraction. Absorption by $Ce^{3+}(^2F_{5/2,7/2}(4f){\rightarrow}^2T_g(5d^1))$, $Co^{2+}(^4A_2(^4F){\rightarrow}^4T_1(^4F)$ or $^4T_1(^4P))$ and $Co^{3+}$, change of ionization energy and lattice parameter were confirmed.

• Journal of the Korean institute of surface engineering
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• v.34 no.5
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• pp.486-493
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• 2001

Partially stabilized zirconia (PSZ) is an attractive material for thermal barrier coating. Zirconia exists in three crystallographic phases: cubic, tetragonal and monoclinic. Especially, the phase transformation of tetragonal phase to monoclinic phase accompanies significant volume expansion, so this transition generally results in cracking and contributes to the failure of the TBC system. Both the plasma sprayed ZrO$_2$-8Y$_2$O$_3$ (YSZ) coat and the ZrO$_2$,-25CeO$_2$,-2.5Y$_2$O$_3$ (CYSZ) coat are isothermally heat -treated at 130$0^{\circ}C$ and 150$0^{\circ}C$ for 100hr and cooled at different cooling rates. The monoclinic phase is not discovered in all the CYSZ annealed at 130$0^{\circ}C$ and 150$0^{\circ}C$. In the 150$0^{\circ}C$ heat-treated specimens, the YSZ contains some monoclinic phase while none exists in the 130$0^{\circ}C$ heat-treated YSZ coat. For the YSZ, the different phase transformation behaviors at the two temperatures are due to the stabilizer concentration of high temperature phases and grain growth. For the YSZ with 150$0^{\circ}C$-100hr annealing, the amount of monoclinic phase increased with the slower cooling rate. The extra oxygen vacancy, thermal stress, and c to t'phase transformation might suppress the t to m martensitic phase transformation.

• Korean Chemical Engineering Research
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• v.40 no.6
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• pp.741-745
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• 2002

Yttria-stabilized zirconia(YSZ) nanopowders were prepared by sol-gel method using zirconium-n-butoxide(ZNB) and yttrium nitrate as precursors. In addition, the effect of water content added during the hydrolysis reaction of ZNB was investigated on the phase composition and pore structure of the product powders. The phase composition of YSZ nanopowders with calcination temperatures showed the same trend, irrespective of $H_2O$ amounts added during the hydrolysis reaction of ZNB. All powders dried at $100^{\circ}C$ were amorphous and transformed to cubic phase at $400^{\circ}C$, which converted to tetragonal phase at $1,000^{\circ}C$. Monoclinic phase also appeared at $1,000^{\circ}C$. The powders showed the mixture of tetragonal and monoclinic phases from $1,000^{\circ}C$ to $1,400^{\circ}C$. The pore size distributions of the dried powders prepared with small amounts of water(less than or equal to $H_2O/ZNB=20$) showed mesopores, while those prepared with large amounts of water(greater than or equal to $H_2O/ZNB=50$) exhibited micropores.

• 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.27 no.3
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• pp.361-368
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• 1990

The properties of the powder of ZrO2＋3m/o Y2O3 system prepared by co-precipitation method at the pH values of 7, 9, 10 and 11 were investigated. ZrOCl2.8H2O and YCl3.6H2O were used as starting materials and NH4OH as a precipitation agent. Zirconium hydroxide near by Zr(OH)4 structure showed more excellent crystallinity and lower formation temperature of tetragonal ZrO2. In the range of this study, cubic ZrO2 was not formed and stability of tetragonal ZrO2 prepared in the conditiion of pH 7 was most excellent. Average particle sizes and specific surface areas of tetragonal ZrO2 powders, prepared as calcining amorphous zirconium hydroxides at $600^{\circ}C$ for 1h, were 0.6-0.8${\mu}{\textrm}{m}$ and 45-70$m^2$/g, respectively.

• Journal of the Korean Ceramic Society
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• v.33 no.5
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• pp.563-571
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• 1996

In order to fabricate solid electrolyte CaO-stabilized ZrO2 of high density sintered body economically 13 mol% CaO-stabilized ZrO2 powders were synthesized by the coprecipitation method. The characteristics and sintering behavior of fine powder were investigated. The precipitates has the specific surface area of 193 m2/g and apperaed to be fine and spherical primary particles with a size of approximately 5nm. The crystalliza-tion temperture of CaO-stabilized ZrO2 was 462$^{\circ}C$. The tetragonal phase was stable in the low calcining tempe-rature regions and the cubic zirconia solid solution was formed from above 120$0^{\circ}C$ through an intermediate stage of formation of CaZrO3 By introducing fine powders washed with alcohol and ball-milling process after calcination the sintered body was possible to attain the value of above 92% of the theoretical density at low temperature of 120$0^{\circ}C$.

• Journal of the Korean Ceramic Society
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• v.23 no.4
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• pp.78-84
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• 1986

Zirconium acetate solution which was obtained from $ZrOCl_2$.$8H_2O$ was condensed polymerized and drawn to fibers by pulling method. Drawn gel fibers fired at 130$0^{\circ}C$ were short porous and mechanically weak. But addition of CaO about 13m/o caused the fibers to have the cubic structure and relatively dense microstructure. In order to clarify the condition for the synthesis of zirconia fibers viscosity measurement DTA-TG analysis X-ray diffraction infrared spectroscopy, SEM and specific surface area were studied.

• Journal of the Korean Ceramic Society
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• v.29 no.2
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• pp.119-126
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• 1992

3 mol% Y2O3-doped ZrO2 powders were prepared by hydrolysis with 0.1, 0.2, 0.3, 0.4, 0.5, 0.6 mol/ιH2O/ethanol into 0.1 mol/ι zirconium and yttrium alkoside/ethanol. Spherical monodispersed yttria-partially stabilized zirconia particles with an average diameter of about 0.5 ${\mu}{\textrm}{m}$ were prepared by hydrolysis with 0.2 mol/ιH2O/ethanol. The as-prepared powder was amorphous and with heating it transformed into cubic up to 80$0^{\circ}C$ and into tetragonal over 100$0^{\circ}C$. 3 mol% Y2O3-doped ZrO2 powders calcined over and up to 80$0^{\circ}C$ were a mixture of tetragonal and monoclinic and only tetragonal as determined by X-ray diffraction, respectively.