• 한국세라믹학회지
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• 제27권2호
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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.

• 한국결정성장학회지
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• 제24권4호
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• pp.140-144
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• 2014

Co(0.7 wt%)와 Pr(2.0, 3.5 및 5.0 wt%)이 첨가된 큐빅지르코니아($ZrO_2:Y_2O_3=50:50wt%$) 단결정을 스컬용융법으로 성장 후 $N_2$ 분위기에서 $1150^{\circ}C$로 5시간 동안 열처리 하였다. 갈색의 단결정들은 각각 어두운 갈녹색, 녹청색 또는 밝은 녹색으로 변화되었다. 열처리 전 후의 YSZ 단결정들을 직경 7.5, 두께 3 mm의 웨이퍼로 연마 하여 UV-VIS 분광광도계 및 XRD(X-ray diffraction)로 광학적 또는 구조적 특성 분석을 행하였다. $Co^{2+}$(약 589 nm: ${\Gamma}_8[^4A_2(^4F)]{\rightarrow}{\Gamma}_8+{\Gamma}_7[^4T_1(^4F)]$, 약 610 nm: ${\Gamma}_8[^4A_2(^4F)]{\rightarrow}{\Gamma}_8[^4T_1(^4F)]$, 약 661 nm: ${\Gamma}_8[^4A_2(^4F)]{\rightarrow}{\Gamma}_6[^4T_1(^4F)]$ 및 $Pr^{3+}$(약 450 nm: ${^3}H{_4}-{^3}P{_2}$, 약 473 nm: ${^3}H{_4}{\rightarrow}{^3}P{_1}$, 약 484 nm: ${^3}H{_4}{\rightarrow}{^3}P{_0}$)에 의한 흡수, 이온화에너지 및 격자상수 변화를 확인하였다.

• 한국결정성장학회지
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• 제22권2호
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• pp.73-77
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• 2012

스컬용융법으로 큐빅지르코니아(YSZ) 단결정들($ZrO_2$: $Y_2O_3$= 80 : 20, 70 : 30, 60 : 40, 50 : 50 wt%, $Co_3O_4$: 0.8wt%, $CeO_2$: 0.4wt%)을 성장시켜 $N_2$ 분위기 $1000^{\circ}C$에서 5시간 동안 열처리 하였다. 오랜지색, 황갈색 또는 갈색의 단결정들은 각각 갈적색, 황색 또는 녹색으로 변화되었다. 열처리 전 후의 YSZ 단결정들은 직경 6.5, 두께 2 mm의 웨이퍼로 연마 하였다. 각 시편의 광학적 또는 구조적 특성은 UV-VIS 분광광도계와 XRD(X-ray diffraction)로 분석하였으며, $Ce^{3+}(^2F_{5/2,7/2}(4f){\rightarrow}^2T_g(5d^1))$, $Co^{2+}(^4A_2(^4F){\rightarrow}^4T_1(^4F)$ 또는 $^4T_1(^4P))$ 및 $Co^{3+}$에 의한 흡수, 이온화에너지 및 격자상수 변화를 확인하였다.

• 한국표면공학회지
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• 제34권5호
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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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• 제40권6호
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• pp.741-745
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• 2002

Sol-Gel법에 의해 출발물질로 zirconium-n-butoxide(ZNB)와 yttrium nitrate를 사용하여 yttria-stabilized zirconia(YSZ) 나노분말을 제조하였다. 또한 ZNB의 가수분해 동안 첨가된 물량의 변화가 얻어진 YSZ 나노분말의 결정상과 기공특성에 미치는 영향을 조사하였다. 하소온도 변화에 따른 결정상 변화는 첨가된 물량에 관계없이 동일한 양상을 보였다. 즉, $100^{\circ}C$에서 건조된 분말은 모두 비정질상이었으며, $400^{\circ}C$에서 입방정상의 결정구조로 전환되었고, $1,000^{\circ}C$에서 정방정상과 단사정상이 나타나 $1,400^{\circ}C$까지 정방정상과 단사정상이 공존하는 결정구조를 보였다. ZNB의 가수분해 중 물의 양이 비교적 적게 첨가된 경우로($H_2O/ZNB=20$이하) 제조된 분말은 mesopore의 기공분포를 보인 반면, 물의 양이 비교적 많이 첨가된 경우에서는 ($H_2O/ZNB=50$이상) micropore의 기공분포를 보였다.

• 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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• 제27권3호
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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.

• 한국세라믹학회지
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• 제33권5호
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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$0^{\circ}C$.

• 한국세라믹학회지
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• 제23권4호
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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.

• 한국세라믹학회지
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• 제29권2호
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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.