• Korean Journal of Materials Research
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• v.10 no.8
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• pp.545-550
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• 2000

3Y-TZP, 12Ce-TZP 및 3Y-TZP, 12Ce-TZP 현탁액의 제타포텐셜과 겉보기점도의 측정으로부터 슬립주입공정에 의한 다층복합체의 제조조건을 조사하였다. 아울러 다층복합체의 소결밀도, 미세구조, 결정상에 미치는 열처리의 영향을 검토하였다. 3Y-TZP와 12Ce-TZP 현탁액의 등전점을 pH 8부근이었으나 3Y-TZP/12Ce-TZP의 등전점은 pH8.6이었다. 현탁액은 전단속도의 증가와 더불어 점도가 감소하는 의가소성유동을 나타내었다. 15 및 20vol% 고체함량을 갖는 3Y-TZP와 3Y-TZP/12Ce-TZP 현탁액은 소량(0.3wt%)의 유기해교제의 첨가만으로 슬립주입에 적당한 유동성을 보유하였으나, 12Ce-TZP의 경우는 점도를 감소시키기 위하여 부가적인 전해질이 필요하였다. 이론밀도의 98% 이상을 보유하고 0.3~$2.2\mu\textrm{m}$의 입경을 갖는 치밀한 다층복합체가$ 1500^{\circ}C$ 소결로 얻어졌다.

• The Korean Journal of Ceramics
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• v.4 no.4
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• pp.297-303
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• 1998

The effect of aliovalent dopants, $ Nb_2O_5$ and MnO, on the phase stability of 12 mol% ceria partially-stabilized zirconia (Ce-TZP) polycrystals was studied. Both dopants (MnO and $ Nb_2O_5$) significantly increased the stability of the tetragonal zirconia phase (Mb temperature lower than liquid nitrogen temperature). The enhancement of the stability of the tetragonal phase in Ce-TZP doped with 1 mol% of Mno(Ce-TZP/MnO) andCe-TZP doped with 1 mol% of $ Nb_2O_5$(Ce-TZP/$ Nb_2O_5$) were explained by the significant reduction of the driving force, -${\Delta}$Gchem, for the tetragonal-to-mono-clinic phase transformation caused by the addition of MnO and $ Nb_2O_5$. The enhanced stability of the tetragonal phase in the Ce-TZP and Al2O3 composite (Ce-TZP/$Al_2O_3$) is believed to be caused by smaller grain size, moderate reduction in the chemical driving force and increase in the strain energy barrier to the transformation. Mechanical properties of the Ce-TZP and the Ce-TZP/$Al_2O_3$ with (i) the same grain size and (ii) the same Mb temperature were examined by measuring stress-strain behavior in 3 point bending. The Ce-TZP/$Al_2O_3$ composite doped with 1.3w% MnO (Ce-TZP/$Al_2O_3$/MnO), which had the same grain size as the Ce-TZP and De-TZP/$Al_2O_3$ showed more transformation plasticity than either the Ce-TZP or the Ce-TZP/$Al_2O_3$ composite. The Ce-TZP wihch had the same Mb temperature as that of the Ce-TZP/$Al_2O_3$/MnO did not show any transformation plasticity.

• 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.36 no.12
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• pp.1390-1395
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• 1999

Zr(Y,Ce)O2 TZP ceramics were prepared by sintering compacts of 3 mol% Y2O3-TZP(3Y-TZP) powders with different amount of 12 mol% CeO2-TZP(12Ce-TZP) in air at 140$0^{\circ}C$ for 2 h. The phase changes microstructure and mechanical properties of Zr(Y. Ce)O2 TZP after hydrothermal aging(20$0^{\circ}C$ 5h) were investigated. Although an addition of 12Ce-TZP accelerated the grain growth of Zr(Y, Ce)O2 TZP it restrained the transformation of tetragonal to the monoclinic phase during aging. The degradation in mechanical properties of sintered bodies was governed by the formed monoclinic phase and chemical composition. Induced Vickers indentation crack was propagated intergranually. From SEM observation of the fracture surfaces the pull-out of individual grain was confirmed.

• Journal of the Korean Ceramic Society
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• v.38 no.5
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• pp.418-423
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• 2001

16 mole%의 CeO$_2$가 고용된 Ce-TZP 소결체 사이에 140~240$mu extrm{m}$ 두께의 Ce-TZP-5~30 vol% $Al_2$O$_3$중간층이 삽입된 층상복합체를 분말건식가압성형법에 의해 제조하였다. 소결온도는 $Al_2$O$_3$가 5~30 vol.% 첨가될 때 90% 이상의 소결밀도를 얻을 수 있도록 1$600^{\circ}C$로 정하였다. 이러한 3층 복합체에서 바깥의 Ce-TZP 지역에서의 파괴 형태는 입내파괴를 보여주었지만 $Al_2$O$_3$가 함유된 중간층에서는 입계파괴가 전이되면서 인성증가를 보여주었다. 이러한 층상 복합체의 경우 중간 층에 들어가는 Ce-TZP 중의 $Al_2$O$_3$함량이 30 vol.% 정도에 이르면 층간의 서로 다른 소결밀도 및 수축율, 열팽창계수 때문에 층간 소결 결함이 생겨 층간에서 균열의 전파가 큰 영향을 받음을 알 수 있었다. 반면 중간층의 $Al_2$O$_3$함량이 적을 경우 층간 결함이 생기지 않아 층간에서 균열의 전파가 별 영향을 받지 않음을 알 수 있었다.

• Korean Journal of Materials Research
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• v.10 no.5
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• pp.321-327
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• 2000

Two kinds of $Al_2O_3/TZP$ composites were prepared using the liquid infiltration of 3Y-TZP and 12Ce-TZP precursors into hte sintered porous $Al_2O_3$. Small TZP additions(~11.0wt%) had increased the strength(19~59%) and fracture toughness(14~157%) of the sintered Al2O3 material($1600^{\circ}C$, 2h). The addition of 3Y-TZP was effective on case of the strength. By the way, in case of the fracture toughness that of 12Ce-TZP was effective. Infiltrated TZP was concentrated on the surface where its grain growth was enhanced and $Al_2O_3$ grain growth was effectively inhibit-ed, when compared to the inner region of the composite. The indentation crack was propagated through both intergranular modes and transgranular and the proportion if intergranular fracture was the larger in $Al_2O_3/12Ce-TZP$.

• Journal of the Korean Ceramic Society
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• v.26 no.5
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• pp.719-727
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• 1989

By using commercial zirconia powder CeO2-ZrO2 ceramics containing 8~16mol% CeO2 was made by heat treatment at 1350~155$0^{\circ}C$ for 1~10hr. The minimum amount of CeO2 for obtaining complete tetragonal phase was 12mol%, and in the tetragonal phase region fracture toughness of Ce-TZP was decreased with increasing CeO2 content and the maximum value was obtained when 12mol% CeO2 was added. The bending strength goes through maximum at 14mol% CeO2. Fracture mode of Ce-TZP transformed from intergranular to transgranular fracture with increasing CeO2 content, so the morphology of fracture surface of 16mol% Ce-TZP was wholly transgranular and this tendency was independent on grain size. The crystal structure of the 12mol% Ce-TZP was monoclinic with fringes along the grain boundaries which are lying in the particular plane from the TEM observation. The chemical composition of the sintered body was homogeneous as a whole and some amorphism or air pocket was observed at the triple junction.

• Journal of the Korean Ceramic Society
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• v.27 no.1
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• pp.55-61
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• 1990

Effect of Al2O3 addition on the mechanical properties and microstructure of Ce-TZP were studied. 12, 14, 16Ce-TZP containing 0-40wt% Al2O3 were prepared by sintering at 155$0^{\circ}C$ for 2h. in air. Density, linear shrinkage, bending strength, Vickers hardness, microstructuer and the amount of stress induced phase transformation were examined. Vickers hardness increased linearly with increasing amounts of Al2O3. The amount of transformation and fracture toughness decreased linearly with increasing amount of Al2O3. Linear shrinkage and relative density decreased with increasing Al2O3 content in all composition of Ce-TZP. Grain growth of Ce-TZP was inhibited by Al2O3 dispersion and fracture mode of Ce-TZP/Al2O3 composites transformed from intergranular to transgranular fracture as the amount of Al2O3 increased. TEM observation revealed that Al2O3 particles were located mainly at grain boundaries of ZrO2.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.10 no.2
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• pp.122-127
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• 2000

Microstructural evolutions in ceria-stabilized zirconia (Ce-TZP) and alumina-dispersed Ce-TZP ceramics were investigated as functions of doping and annealing conditions. All of sintered specimens showed the relative density over 99 %. Sintered specimens had linear grain boundaries and normal grain shapes, but ceria-doped specimens had irregular grain shapes and nonlinear grain boundaries due to the diffusion-induced grain boundary migration during annealing at $1650^{\circ}C$ for 2 h. Mean grain boundary length of Ce-TZP with irregular grain shapes was higher than that of normal grain shapes, and was a value of 23pm at the maximum. Alumina particles dispersed in Ce-TZP inhibited the grain growth of zirconia particles. $Al_2O_3$Ce-TZP doped with ceria and annealed at $1650^{\circ}C$ for 2 h showed irregular grain shapes as well as small grain size. Added alumina particles showed the grain growth during sintering or annealing, and they changed the position from grain boundary to inside of the grains during the annealing. The specimens with normal grain shapes showed an intergranular fracture mode, whereas the specimens with irregular grain shapes showed a transgranular fracture mode during the crack propagation.

• The Korean Journal of Ceramics
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• v.5 no.1
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• pp.1-11
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• 1999

The effect of aliovalent dopents, $Nb_3O_5$ and MnO, on the grain growth kinetics of 12 mol% ceria stabilized tetragonal zirconia polycrystals (Ce-TZP) was studied. All specimens were sintered at $1550^{\circ}C$ for 20 minutes prior to annealing at different temperatures to study grain growth kinetics. Grain growth kinetics of Ce-TZP and 1 mol% $Nb_2O_5$ doped Ce-TZP (Ce-TZP/$Nb_3O_5$) during annealing at 1475, 1550, and $1600^{\circ}C$ adequately matched with square law $(D^2-D_\;o^2=k_at)$. However, grain growth in 1 mol% MnO suppressed grain growth in Ce-TZP by drag force exerted by $Mn^{+2}$ ions which segregated strongly to the positively-charged grain boundaries of Ce-TZP, $Nb_2O_5$ enhanced grain growth by increasing the concentration of vacancies of $Zr^{+4}$ ion and $Ce^{+4}$ ions. Surface analysis with X-ray photoelectron spectroscopy (XPS) showed the segregation of Mn+2 ions to grain boundaries. The kinetics of grain growth obtained in the base Ce-TZP and the Ce-TZPs with the aliovalent dopants were examined in the context of impurity drag effect and space charge effect.