• 한국재료학회지
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• 제10권8호
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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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• 제4권4호
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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.

• 한국세라믹학회지
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• 제33권10호
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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.

• 한국세라믹학회지
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• 제36권12호
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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.

• 한국세라믹학회지
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• 제38권5호
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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.

• 한국재료학회지
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• 제10권5호
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• pp.321-327
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• 2000

다공성 알루미나 소결체내부로 3Y-TZP 및 12Ce-TZP 전구체를 각각 액상침투시킴으로써 2종류의 $Al_2O_3/TZP$복합체를 제조하였다. 소량의 (~11.0 wt%) TZP의 첨가는 Al2O3소결체 ($1600^{\circ}C$, 2시간)의 강도 (19~59%)와 파괴인성(14~157%)을 증가시켰다. 3Y-TZP의 첨가는 복합체의 강도의 향상에 12Ce-TZP의 첨가는 인성의 향상에 보다 효과적이었다. 침투도니 TZP는 복합체의 내부보다 표면에 집중되었으며, 그 결과 이곳에서의 입성장에 빨랐고 $Al_2O_3$의입성장 억제효과도 상대적으로 뛰어났다. 입계 및 입내균열전파가 일어났으나 $Al_2O_3/12Ce-TZP$의 경우가 $Al_2O_3/3Y-TZP$에 비하여 입계파괴가 우세하였다

• 한국세라믹학회지
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• 제26권5호
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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.

• 한국세라믹학회지
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• 제27권1호
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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.

• 한국결정성장학회지
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• 제10권2호
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• pp.122-127
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• 2000

불규칙 입자형성을 갖는 Ce-TZP와 알루미나가 분산된 Ce-TZP 세라믹스를 세라아 도핑조선과 열처리 조건을 변화시켜 제조한 다음, 미세구조를 관찰하였다. 제조된 시편들은 상대밀도가 99% 이상인 고밀도의 소결체였으며, 정방정 및 입방정상 지르코니아 입자로 구성되었다. 도핑하지 않거나 소결만 시킨 시편의 경우 직선적인 입계와 정상적인 입자형성을 나타낸데 비하여 세리아를 침적법으로 도핑한 후 고온으로 열처리한 시편에서는 확산구동 입계이동이 일어나 입계 및 입자형성이 불규칙하였으며. 이러한 Ce-TZP에서는 입자당 평균 입계같이 정상입자에 비하여 크게 증가하였다. 알루미나를 분산시켜 소결한 {{{{ { Al}_{2 }{ O}_{3 } }}}}/Ce- TZP 시편의 경우, 알루미나 입자에 의해서 입성장이 크게 억제되었고, 세리아를 도핑한 후 소결과 열처리를 행한 {{{{ { Al}_{2 }{ O}_{3 } }}}}/Ce-TZP에서는 불규칙 입자형상이 형성되면서도 입성장이 억제되어 입자크기에 비하여 입계면적이 크게 증가하였다. 분산된 알루미나 입자들은 소결과 열처리 과정 중 입자크기가 증가하였고, 열처리 동안 많은 입자들이 입계에서 입내로 위치가 변화하였다. 정상적인 입자형성을 갖은 시편에서는 균열진전시 입계파괴가 주로 일어났으나 불규칙 입자형성을 갖는 시편에서는 주로 입내파괴가 관찰되었다.

• The Korean Journal of Ceramics
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• 제5권1호
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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.