• The Korean Journal of Ceramics
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• v.1 no.4
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• pp.214-218
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• 1995

Partially stabilized zironia with magnesia (Mg-PSZ) is known as one of the toughest monolithic ceramics. However, the very large grain sizes obtained after sintering at a high solution-heat treatment temperature in the cubic region of the phase diagram limit the strength of this material rather modest. In this study fine-grained Mg-PSZ materials were fabricated by adding TiC particles as a dispersed phase. Samples were hot-pressed at $1750^{\circ}C$ and then annealed at $1420^{\circ}C$ for various times. Grain growth was retarded severely by the TiC particles resulting in grain sizes smaller by more than one order of magnitude than those of PSZ without TiC. The fine-grained microstructure lead to doubly-increased fracture strength while maintaining the same level of high fracture toughness as that of conventional Mg-PSZ without TiC particles.

• The Korean Journal of Ceramics
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• v.2 no.2
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• pp.102-110
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• 1996

The Mg-PSZ/$Al_2O_3$ fibers were fabricated by the sol-gel method. The added $Al_2O_3$ amounts were varied from 5 to 20 mol%. The phase transformation studies of a drawn Mg-PSZ/$Al_2O_3$ fibers were investigated by use of X-ray diffraction, IR and Raman spectroscopy. Microstructure and tensile strength of fibers were subjected to scanning electron microscopy and tensile strength tester. When $Al_2O_3$ was added to the Mg-PSZ fibers, it was found out from the analysis of XRD patterns and Raman spectra that a small amount of crystalline spinel($MgAl_2O_4$) started to form due to the reaction between $Al_2O_3$ and MgO, at $1000^{\circ}C$, and the phase transformation temperature of $ZrO_2$ crystal phase at different sintering temperatures increased. Also, the rapid grain growth with average size of 2.0 ${\mu}m$ shown in Mg-PSZ fiber at $1500^{\circ}C$ was considerably suppressed to 0.39 ${\mu}m$ by adding $Al_2O_3$ at the same temperature. When the Mg-PSZ/$Al_2O_3$ fibers containing 5 mol% $Al_2O_3$ were sintered $800^{\circ}C$ for 1 hr, average tensile strength of fibers was 0.9 GPs at diameters of 20 to 30 ${\mu}m$, but as the sintering temperatures was increased to $1000^{\circ}C$ for 1 hr, average tensile strength of fibers increased to 1.2 GPa in the same diameter range.

• Journal of the Korean Ceramic Society
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• v.31 no.6
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• pp.651-659
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• 1994

BaTiO3 ceramics were sintered on Al2O3, MgAl2O4, MgO and Mg-, Ca-, Y-stabilized zirconia setters. Then the influence of setters on the microstructure of BaTiO3 ceramics and the stability of setters were investigated by SEM, EDAX and XRD analyses. The microstructure of BaTiO3 ceramics sintered on Al2O3, MgAl2O4, MgO and Mg-PSZ showed large grain growth, but little grain growth on Ce-TZP(Tetragonal Zirconia Policrystal). Mg-PSZ(Partially Stabilized Zirconia), Ca-PSZ, Ce-TZP setters showed extensive phase transformation. Y-TZP and fused Y-SZ (Stabilized Zirconia) setters were stable. The liquid sintering aids of BaTiO3 ceramics accelerate mass transport. The reaction of SrTiO3 in BaTiO3 with ZrO2 resulted in the formation of SrZrO3.

• Journal of the Korean Ceramic Society
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• v.24 no.3
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• pp.243-250
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• 1987

The effects aging on some properties and thermal-shock behavior of zirconia partially stabilized with 9 mol% MgO (9MZ) were studied. 9MZ specimens were aged over $1200^{\circ}$-$1400^{\circ}C$ for 12hours subsequently, after sintering at $1650^{\circ}C$ for 4 hours. Fracture strength(both before and after thermal-shock test), linear thermal expansion, monoclinic fraction and phase transition by XRD, density, galvanic potential and microstructure were measured. Quantitative chemical analysis around the grain-boundary of the specimen aged at $1350^{\circ}C$ was also conducted by EDX. The aging of 9MZ specimen causes a thermal decomposition of cubic-$ZrO^{2}$ into the formation metastable tetragonal-$ZrO^{2}$ and MgO. The former increases the residual strength after thermal-shock test and the latter improves the thermal-shock resistance due to thermal conduction through the continuous magnesia phase and the formation of monoclinic phase content in matrix were increased with decreasing the aging temperature from $1400^{\circ}C$ to $1200^{\circ}C$. Galvanic potential of the aged specimen exhibited a proper emf characteristic.

• Journal of Sensor Science and Technology
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• v.18 no.6
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• pp.441-448
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• 2009

Magnesia partially stabilized zirconia(Mg-PSZ) solid electrolytes for an improvement of thermal shock resistance, which is suitable for the measurement of oxygen activity in a molten steel, were prepared by post-thermal aging treatment. The steelmaking oxygen sensor elements were formed by an injection molding method, sintered at $1650^{\circ}C$, and then thermal aged ranged from 1250 to $1400^{\circ}C$. Sintered density and porosity were decreased as increasing the magnesia content in a zirconia-magnesia solid solution. Fractions of cubic phase to the synthesized Mg-PSZ solid electrolytes were ranged from 13.13 to 79.54.% after post-thermal aging treatment. Very dense microstructure without voids in the grains was obtained by the post-thermal aging process. Fine tetragonal phase crystallites precipitated on the cubic surface during post-thermal aging up to $1300^{\circ}C$ improve a thermal shock resistance and reappearance of electro motive force(EMF) curve.

• Journal of the Korean Ceramic Society
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• v.25 no.2
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• pp.131-135
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• 1988

The microstructural changes in partially stabilized MgO-ZrO2 alloys during heat treatment and mechanical properties of ZrO2(Y2O3)/Al2O3 systems have been studied. 9mol% MgO-ZrO2 powders were sintered at 1800$^{\circ}C$ for 4 hours and these specimens were aged at 1420$^{\circ}C$ and 1100$^{\circ}C$ secondly. These specimens have high thermal shock resistance and high toughness. The bend strength of Y-PSZ/Al2O3 composites conventially sintered were increased by HIP from 650MPa to 980MPa.

• Proceedings of the Korea Association of Crystal Growth Conference
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• 1996.06b
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• pp.55-85
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• 1996

지르코니아 분말은 ZrO2 결정상이 온도변화에 따라 부피변화를 수반하는 상전이변태를 나타낸다. 단사정 ZrO2가 110$0^{\circ}C$에서는 정방정으로, 2$700^{\circ}C$ 내외에서는 입방정으로 결정구조가 가역적으로 변한다. 이 ZrO2에 금속산화물을 고용시키면 형석 (CaF2:Florite)형의 입방정 결정구조가 실온에서도 안정하게 존재하게 된다. 안정화제 산화물은 caO, MgO등 2가 산화물외에 3가 또는 4가의 금속산화물로서 Sc2O3, Y2O3, Sm2O3, Nd2O3, Gd2O3, Y2O3, CeO2 등이며 이들은 금속이온의 원자가가 변하기 쉬운 희토류 산화물이다. 안정화 지르코니아는 형석형 결정구조이며 결정화학적으로 보면 금속양이온이 산소이온에 대해서 정육면체형의 8배위를 하고 있다. 이때 이온반경비(양이온/음이온)에 따라 Zr+4자리와 O-2자리의 격자위치와 모양이 형성되므로 비틀어진 정육면체구조이건 이상적인 정육면체 형석구조를 이룬다. 이는 지르코니아의 결정상의 2상-3상인 부분안정화 지르코니아다결정체(PSZ : partially stabilized zirconia)이거나 단일상-2상인 정방정 지르코니아다결정체(TZP : tetragonal zirconia polycrystal)의 결정구조를 가지는데 기인한다. PSZ는 주로 MgO, CaO를 안정화제로 고용시켜 입방정 영역에서 소결하고 이를 다시 입방정과 정방정의 상 영역에서 열처리하여 입방정 입자내부에 정방정을 석출 형성시킨 것이며 TZP는 Y2O3 및 CeO2를 고용시켜 PSZ와 다르게 일반적인 상압소결한 정방정 결정상의 미립자이다. 산화지르코늄 분말은 지르콘사에서 열분해시킨 지르코늄소결.융해괴(caustic fusion clinker)를 산처리하여얻어진 지르코늄산용액(zirconyl acid solution : cloride, sulfide, nitride 등)으로부터 제조된다. 고순도 산화지르코늄은 용액 결정석출법에 의해 ZrOCl2.8H2O, 5ZrO2.3SO3.15H2O, ZrO(NO3)2.xH2O 등의 지르코늄 수화물만을 재결정화시킨 것으로부터 얻을 수 있으며 이 지르코늄염 수용액으로부터 입자미세구조를 효과적으로 제어하여 산화지르코늄 및 안정화 지르코니아 분말제조가 가능하다. 안정화 지르코니아 분말은 ZrO2와 안정화산화물의 고용을위하여 가열처리를 필요로 하며 일정온도에서 최적상태로 숙성하므로서 2가지 상(phase) 이상의 고용체를 가지게 된다. 안정화 지르코니아 분말은 고용처리온도를 낮추고 효과적으로 생성시키기 위해서는 지르코늄 및 안정화제염을 혼합하고 습식 직접합성하여 저온에서 고용체의 합해진상 영역을 생성시키는 것이다. 이는 지르코니아 원료분말의 미세구조를 제어하므로서 가능하며 이때 화학성분조성과 크기형태가 균일하게 분포된 입자분말을 얻을 수 있다.