• Korean Journal of Materials Research
• /
• v.7 no.5
• /
• pp.411-416
• /
• 1997

수소 및 산소분위기 하에서 2Y-TZP 및 3Y-PZP 세라믹스를 소결하여 각각 제조한 다음, 각 시편의 미세구조 및 25$0^{\circ}C$에서의 등온상전이 거동을 비교하여 고찰하였다. 그 결과 수소분위기에서 소결한 모든 시편의 표면에서는 Zr$_{4+}$ 이온의 환원에 의해 산화분위기에서 소결한 시편에 비하여 색이 검게 변하였으며, 장시간 소결시 시편 표면에 조대 입자의 생성 및 입계 이완이 관찰되었다. 이에따라 수소분위기 하에서 장시간 소결된 시편의 경우 냉각 시 상전이가 일어나 다량의 단사정상이 상온에서 존재하였다. 저온 aging동안 등온상전이 속도는 산소분위기에서 소결한 시편보다 수소분위기에서 소결한 시편에서 낮게 나타났으며, 이러한 경향은 $Y_{2}$O$_{3}$의 고용량이 크고, 입자크기가 적은 시편일수록 증가하였다. 또한 2Y-TZP 시편에서는 입자크기에 상관없이 대부분의 정방정상이 단사정상으로 빨리 등온상전이를 일으켰으나, 3Y-TZP 시편의 경우, 등온상전이는 입자크기가 증가함에 따라 상전이 속도도 증가하였다.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.12 no.3
• /
• pp.126-132
• /
• 2002

The nanocrystalline zirconia powder with anisotropic shapes was synthesized by hydrothermal treatment of the tetragonal zirconia prepared by aging the zirconium hydroxide precipitate, which was obtained from the reaction between $ZrOCl_2{\cdot}8H_2O$ and KOH solutions under the fixed pH of 13.5, at $100^{\circ}C$ for 24 h. With increasing the hydrothermal reaction temperature and time, the fraction of tetragonal phase with spherical zirconia decreased, whereas, relatively the fraction of monoclinic phase with spindle-like and rod shape zirconia increased. As increased concentration of the NaOH solution it promoted the particle size to become larger and the crystalline phase to transform tetragonal to monoclinic. However, the specific surface area at the early stage of the reaction increased and subsequently decreased because of grain growth in powder with longer reaction time.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.2 no.2
• /
• pp.63-70
• /
• 1992

$AI_2O_3/Ca-TZP$ composites was prepared by using the starting powder of alumina and Ca-TZP synthesized by hydrothermal reaction and investigated to its characteristics. The ratio of tetragonal zirconia to monoclinic within $AI_2O_3$ matrix was decreased with an addition of Ca-TZP content, but the absolute amount of tetragonal phase in composites was increased with an addition of Ca-TZP content. The value of fracture toughness in $AI_2O_3/Ca-TZP$composites was proportional to the amounts of transformed tetragonal phase which formed by crack propagation in fracture, and therefore, it was gradually increased with an addition of Ca- TZP content.

• Journal of the Korean Ceramic Society
• /
• v.37 no.9
• /
• pp.856-863
• /
• 2000

상압 소결법과 통전활성 소결(Plasma Activated Sintering; PAS)법으로 120$0^{\circ}C$부터 150$0^{\circ}C$의 온도범위에서 제조된 지르코니아의 기계적 특성을 ring on ring disk 굽힘시험으로 비교하여 고찰하였다. 모든 소결온도범위에서 PAS법으로 제조된 소결체의 밀도와 경도는 상압 소결법에 의해 제조된 소결체 보다 높게 나타났다. 결정립의 크기는 두 소결법에 의해 제조된 소결체 모두에서 소결온도 증가에 따라 증가하였으나, PAS법으로 제조된 소결체가 상압 소결법으로 제조된 소결체 보다는 결정립 성장이 억제되었다. 파괴인성은 PAS법으로 제조된 소결체의 경우 130$0^{\circ}C$에서 최고값을 나타낸 후 소결온도 증가에 따라 미세하게 감소하였으며, 상압 소결법으로 제조된 소결체의 경우 소결온도 증가에 따라 증가되었다. 소결체의 상분율 변화는 PAS법으로 제조된 경우 전 온도범위 (1200~150$0^{\circ}C$)에서 정방정상만 관찰되었으며, 상압 소결법의 경우 단사정상과 정방정상의 혼합상을 나타내었고, 소결온도 증가에 따라 정방정상의 비율이 증가하였다. 결과적으로 PAS법의 경우 지르코니아의 최적 소결온도는 130$0^{\circ}C$이며, 상압 소결법의 경우 150$0^{\circ}C$임을 알 수 있었으며, 소결체의 파괴인성에 미치는 영향은 결정립 크기 및 정방정상의 분율임을 확인할 수 있었다.

• Korean Chemical Engineering Research
• /
• v.40 no.6
• /
• pp.741-745
• /
• 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 Mineralogical Society of Korea
• /
• v.19 no.2 s.48
• /
• pp.81-88
• /
• 2006

The Yttria Partially Stabilized Zirconia powder was prepared by spontaneous precipitation method using $ZrOCl_2{\cdot}8H_O-YCl_33{\cdot}6H_2O$ solution as a starting materials. The optimal experimental conditions such as concentration and pH of starting solutions, the amounts of stabilizer $Y_2O_3$ used, and sintered temperature were carefully studied. The best condition for synthesizing $ZrO_2$ was experimentally selected and applied throughout this study for the preparation of the 3 mole% $Y_2O_3$ partially stabilized zirconia, 3YSZ. The physical properties of 3YSZ was examined by XRD, Raman, DT A, and SEM. The structural transition from pure monoclinic high temperature $ZrO_2$ to tetragonal room temperature 3YSZ was made possible by the added amount of $Y_2O_3$ in the $ZrO_2+Y_2O_3$ system. All Raman Spectrum band appeared in the lower wave numbers rather than in higher wave numbers as structure changes from monoclinic to tetragonal.

• Korean Journal of Materials Research
• /
• v.2 no.5
• /
• pp.320-329
• /
• 1992

In 2Y-TZP powders calcined at temperature range of 80$0^{\circ}C$0 to 150$0^{\circ}C$, the effect of stabilization and the transformability of tetragonal phase on the tetragonal to monoclinic transformation have been investigated. The transformability of tetragonal phase in calcined powders shows maximum at the calcination temperature of 130$0^{\circ}C$. This result is explained by a combined effect of the increase of particle size and of constrained force among the particles with increasing the calcination temperature. The amount of transformed monoclinic phase with calcination temperature after quenching in liquid nitrogen, stress induction and isothermal aging at 25$0^{\circ}C$is also explained by the transformability of tetragonal phase determined by the sum of particle size effect and constraint effect.

• Journal of the Korean Ceramic Society
• /
• v.33 no.6
• /
• pp.637-644
• /
• 1996

Phase stability and isothermal phase transformation during gaging at 25$0^{\circ}C$ were investigated in yttria stabilized zirconia powders prepared from hydrolysis of zirconium isopropoxide. The stability of tetragonal phase at room temperature in zirconia powder was decreased with calcination temperature but increased with the addition of yttria content. During aging at 25$0^{\circ}C$ in humid atmosphere isothermal phase transformation occurred in tetragonal zirconia powder stabilized by constraint effect not by alloying effect and grain size effect. Many twins and microcrackings were found in transformed monomlinic zirconia particles.

• Journal of the Korean Ceramic Society
• /
• v.25 no.3
• /
• pp.225-230
• /
• 1988

The strength and thermal shock resistance of $Al_2O_3-ZrO_2$ composites have been studied. The tetragonal $ZrO_2$ powder containing 1 mol.% $Y_2O_3$ and monoclinic $ZrO_2$ powder were prepared by coprecipitation method and subsequently mixed with $Al_2O_3$ powder and granulated by sieving. Duplex composites were prepared by dry mixing matrix agglomerate with 15 to 30 vol.% of dispersion agglomerate, followed by pressing and sintering at 1$600^{\circ}C$ for1 hr. These $Al_2O_3-ZrO_2$ 2 composites having heterogeneous structure showed improved thermal shock behaviors because of the microcracking and pores in dispersed granules, and compressive stresses around dispersed granules resulting from $ZrO_2$ transformation.

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